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ASM

INTERNATIONAL ®

Publication Information and Contributors

Materials Characterization printing (1992), the series title was changed to was published in 1986 as Volume 10 of the 9th Edition ASM Handbook. The Volume was prepared under the direction of the Metals Handbook. With the third

ASM Handbook Committee.

Volume Coordinator

The Volume Coordinator was Ruth E. Whan, Sandia National Laboratories.

Organizing Committee

• • Rafael Menezes NunesRuth E. Whan Chairman UFRGS Sandia National Laboratories
• • Ray W. CarpenterPaul T. Cunningham Arizona State UniversityLos Alamos National Laboratory
• • William H. DingledeinKenneth H. Eckelmeyer Carpenter Technology CorporationSandia National Laboratories
• • Dean A. FlinchbaughRaymond P. Goehner Bethlehem Steel CorporationSiemens Corporation
• • J.I. GoldsteinMerton Herrington Lehigh University Special Metals
• • Harris L. MarcusCarolyn McCrory-Joy University of Texas AT&T Bell Laboratories
• • David A. SmithSuzanne H. Weissman IBM Thomas J. Watson Research Center Sandia National Laboratories

Authors and Reviewers

• • Brent L. AdamsR.W. Armstrong Brigham Young UniversityUniversity of Maryland
• • Mark A. ArnoldRoger A. Assink University of IowaSandia National Laboratories
• • Raghavan AyerDelbert S. Berth Exxon Research & Engineering CompanyUniversity of Nevada
• • Larry H. BennettS.M. Bhagat University of Maryland National Bureau of Standards
• • J.C. BilelloJack Blakely State University of New York at Stony BrookCornell University
• • George A. BlannG. Dana Brabson Buehler Ltd.University of New Mexico
• • S.S. BrennerChris W. Brown University of Pittsburgh University of Rhode Island
• • Elliot L. BrownD.R. Browning ConsultantColorado School of Mines
• • Richard R. BuckRobert W. Buennecke University of North Carolina Caterpillar Tractor Company
• • Merle E. BunkerFrank B. Burns Sandia National LaboratoriesLos Alamos National Laboratory
• • Thomas A. CahillAlan Campion University of Texas--Austin University of California--Davis
• • Martin J. CarrJoel A. Carter Oak Ridge National LaboratorySandia National Laboratories
• Anders Cedergren University Umea

• • T.J. HeadleyG. Heath University of Edinburgh Sandia National Laboratories
• • Kurt F.J. HeinrichMichael B. Hintz Michigan Technological UniversityNational Bureau of Standards
• • Paul F. HlavaPaul Ho IBM Thomas J. Watson Research Center Sandia National Laboratories
• • David H. HuskissonHatsuo Ishada Case Western Reserve University Sandia National Laboratories
• • Michael R. JamesA. Joshi Lockheed Palo Alto Research Laboratory Rockwell International Science Center
• • Silve KallmannJ. Karle Naval Research Laboratory Ledoux and Company
• • Michael J. KellyLowell D. Kispert Sandia National LaboratoriesUniversity of Alabama
• • David B. KnorrJohn H. Konnert Olin CorporationNaval Research Laboratory
• • Jiri KorytaByron Kratochvil Czechoslovak Academy of Sciences University of Alberta
• • Aaron D. KrawitzG.R. Lachance Geological Survey of Canada University of Missouri--Columbia
• • Max G. LagallyD.G. LeGrand General Electric CompanyUniversity of Wisconsin
• • Donald E. LeydenEric Lifshin General Electric R&D Center Colorado State University
• • J.S. LinMacIntyre R. Louthan, Jr. Oak Ridge National Laboratory Virginia Polytechnic Institute and State University
• • Jesse B. LumsdenC.E. Lyman Lehigh University Rockwell International Science Center
• • Curtis MarcottJ.L. Marshall Oak Ridge Y-12 PlantThe Proctor & Gamble Company
• • George M. MatlackJames W. Mayer Cornell UniversityLos Alamos National Laboratory
• • M.E. McAllasterGregory J. McCarthy Sandia National Laboratories North Dakota State University
• • Linda B. McGownN.S. McIntyre University of Western Ontario Oklahoma State University
• • T. MehrhoffD.M. Mehs Fort Lewis CollegeGeneral Electric Neutron Devices
• • Louis MeitesC.A. Melendres George Mason University Argonne National Laboratory
• • Raymond M. MerrillM.E. Meyerhoff University of Michigan Sandia National Laboratories
• • J.R. MichaelA.C. Miller Alcoa Technical CenterBethlehem Steel Corporation
• • Dennis MillsM.M. Minor Cornell UniversityLos Alamos National Laboratory
• • Richard L. MooreGerald C. Nelson Sandia National LaboratoriesPerkin-Elmer Corporation
• • Dale E. NewburyJohn G. Newman National Bureau of StandardsPerkin-Elmer Corporation
• • Monte C. NicholsM.A. Nicolet California Institute of Technology Sandia National Laboratories
• • M.R. NotisM.C. Oborny Lehigh UniversitySandia National Laboratories

• • John OlesikMark Ondrias University of North CarolinaUniversity of New Mexico
• • David G. OneyRobert N. Pangborn Cambridge Instruments Inc. Pennsylvania State University
• • Carlo G. PantanoJeanne E. Pemberton Pennsylvania State University University of Arizona
• • William M. PetersonBonnie Pitts LTV Steel Company EG&G Princeton Applied Research Corporation
• • Charles P. Poole, Jr.Ben Post Polytechnic Institute of New York University of South Carolina
• • Paul S. PreveyWilliam C. Purdy Lambda Research, Inc. McGill University
• • R. RametteLeo A. Raphaelian Carleton College Argonne National Laboratory
• • Julian L. Roberts, Jr.Philip J. Rodacy Sandia National Laboratories University of Redlands
• • Alton D. Romig, Jr.Fred K. Ross University of Missouri Research Reactor Sandia National Laboratories
• • James F. RuslingAlexander Scheeline University of Connecticut University of Illinois at Urbana-Champaign
• • Jerold M. SchultzW.D. Shults Oak Ridge National Laboratory University of Delaware
• • Darryl D. SiemerJohn R. Sites Oak Ridge National Laboratory Westinghouse Idaho Nuclear Company
• • Deane K. SmithG.D.W. Smith University of OxfordPennsylvania State University
• • Robert SmithWalter T. Smith, Jr. Allied Bendix Corporation University of Kentucky
• • Robert L. SolskyW.R. Sorenson Sandia National LaboratoriesE.I. DuPont de Nemours & Co., Inc.
• • John SpeerRichard S. Stein Bethlehem Steel Company University of Massachusetts
• • John T. StockR. Sturgeon National Research Council of CanadaUniversity of Connecticut
• • L.J. SwartzendruberJohn K. Taylor National Bureau of Standards National Bureau of Standards
• • L.E. ThomasM.T. Thomas Westinghouse Hanford CompanyBattelle Pacific Northwest Laboratory
• • Maria W. TikkanenThomas Tombrello California Institute of TechnologyApplied Research Laboratory
• • Ervin E. UnderwoodJames A. VanDenAvyle Georgia Institute of TechnologySandia National Laboratories
• • David L. VanderhartJohn B. Vander Sande National Bureau of StandardsMassachusetts Institute of Technology
• • George F. Vander VoortK.S. Vargo Sandia National Laboratories Carpenter Technology Corporation
• • John D. VerhoevenL. Peter Wallace Lawrence Livermore National LaboratoryIowa State University
• • I.M. WarnerJohn Warren Emory UniversityEnvironmental Protection Agency
• • E.L. WehrySigmund Weissman University of Tennessee Rutgers, The State University of New Jersey
• • Suzanne H. WeissmanOliver C. Wells IBM Thomas Watson Research Center Sandia National Laboratories

• • John W. PridgeonRaymond F. Decker President and TrusteeVice President and Trustee Consultant Michigan Technological University
• • M. Brian IvesFrank J. Waldeck Immediate Past President and Trustee Treasurer Lindberg Corporation McMaster University

Trustees

• • Herbert S. KalishWilliam P. Koster Adamas Carbide CorporationMetcut Research Associates, Inc.
• • Robert E. LuetjeRichard K. Pitler Armco, Inc.Allegheny Ludlum Steel Corporation
• • Wayne A. ReinschC. Sheldon Roberts TimetConsultant Materials and Processes
• • Gerald M. SlaughterWilliam G. Wood Technology Materials Oak Ridge National Laboratory
• • Klaus M. ZwilskyEdward L. Langer National Materials Advisory BoardManaging Director National Academy of Sciences

Members of the ASM Handbook Committee (1985-1986)

• Thomas D. Cooper Laboratories (Chairman 1984-; Member 1981-) Air Force Wright Aeronautical
• • Roger J. AustinDeane I. Biehler (1984-)(1984-) Materials Engineering ConsultantCaterpillar Tractor Company
• • Thomas A. FreitagCharles David Himmelblau (1985-) (^) (1985-)The Aerospace Corporation Lockheed Missiles & Space Company, Inc.
• • John D. HubbardDennis D. Huffman (1984-) (1983-) HinderTec, Inc.The Timken Company
• • Conrad MitchellDavid LeRoy Olson (1983-) (1982-) United States Steel Corporation Colorado School of Mines
• • Ronald J. RiesPeter A. Tomblin (1983-) (1985-) The Timken CompanyDeHavilland Aircraft of Canada
• • Derek E. TylerLeonard A. Weston (1983-) (1982-) Olin Corporation Lehigh Testing Laboratories, Inc.

Previous Chairmen of the ASM Handbook Committee

• • R.S. ArcherL.B. Case (1931-1933) (Member, 1927-1933)(1940-1942) (Member, 1937-1942)
• • E.O. DixonR.L. Dowdell (1952-1954) (Member, 1947-1955)(1938-1939) (Member, 1935-1939)
• • J.P. GillJ.D. Graham (1937) (Member, 1934-1937) (1966-1968) (Member, 1961-1970)
• • J.F. HarperC.H. Herty, Jr. (1923-1926) (Member, 1923-1926) (1934-1936) (Member, 1930-1936)
• • J.B. JohnsonL.J. Korb (1983) (Member, 1978-1983)(1948-1951 ) (Member, 1944-1951)
• • R.W.E. LeiterG.V. Luerssen (1962-1963) (Member, 1955-1958, 1960-1964)(1943-1947) (Member, 1942-1947)
• • Gunvant N. ManiarJames L. McCall (1982) (Member, 1977-1982)(1979-1980) (Member, 1974-1980)
• W.J. Merten (1927-1930) (Member, 1923-1933)

• • N.E. PromiselG.J. Shubat (1973-1975) (Member, 1966-1975)(1955-1961) (Member, 1954-1963)
• • W.A. StadtlerRaymond Ward (1969-1972) (Member, 1962-1972)(1976-1978) (Member, 1972-1978)
• • Martin G.H. WellsD.J. Wright (1964-1965) (Member, 1959-1967) (1981) (Member, 1976-1981)

Staff

ASM International staff who contributed to the development of the Volume included Kathleen Mills, Manager ofEditorial Operations; Joseph R. Davis, Senior Technical Editor; James D. Destefani, Technical Editor; Deborah A.

Dieterich, Production Editor; George M. Crankovic, Assistant Editor; Heather J. Frissell, Assistant Editor; and Diane M.Jenkins, Word Processing Specialist. Editorial assistance was provided by Esther Coffman, Robert T. Kiepura, and

Bonnie R. Sanders. The Volume was prepared under the direction of William H. Cubberly, Director of Publications; andRobert L. Stedfeld, Associate Director of Publications.

Conversion to Electronic Files

ASM Handbook based on the Fifth printing (1998). No substantive changes were made to the content of the Volume, but some minor, Volume 10, Materials Characterization was converted to electronic files in 1998. The conversion was

corrections and clarifications were made as needed.

ASM International staff who contributed to the conversion of the Volume included Sally Fahrenholz-Mann, BonnieSanders, Marlene Seuffert, Gayle Kalman, Scott Henry, Robert Braddock, Alexandra Hoskins, and Erika Baxter. The

electronic version was prepared under the direction of William W. Scott, Jr., Technical Director, and Michael J.DeHaemer, Managing Director.

Copyright Information (for Print Volume)

Copyright © 1986 ASM International

All rights reserved

No part of this book may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means,electronic, mechanical, photocopying, recording, or otherwise, without the written permission of the copyright owner.

First printing, June 1986

Second printing, October 1988

Third printing, February 1992

Fourth printing, January 1996

Fifth printing, March 1998

ASM Handbook is a collective effort involving thousands of technical specialists. It brings together in one book a wealthof information from world-wide sources to help scientists, engineers, and technicians solve current and long-range

problems.

Great care is taken in the compilation and production of this volume, but it should be made clear that no warranties,express or implied, are given in connection with the accuracy or completeness of this publication, and no responsibility

can be taken for any claims that may arise.

Nothing contained in the ASM Handbook shall be construed as a grant of any right of manufacture, sale, use, orreproduction, in connection with any method, process, apparatus, product, composition, or system, whether or not covered

Introduction to Materials Characterization R.E. Whan, Materials Characterization Department, Sandia National Laboratories

Scope

Materials Characterization background in materials analysis with an easily understood reference book on analytical methods. Although there is an has been developed with the goal of providing the engineer or scientist who has little

abundance of excellent in-depth texts and manuals on specific characterization methods, they frequently are too detailedand/or theoretical to serve as useful guides for the average engineer who is primarily concerned with getting his problem

solved rather than becoming an analytical specialist. This Handbook describes modern analytical methods in simplifiedterms and emphasizes the most common applications and limitations of each method. The intent is to familiarize the

reader with the techniques that may be applied to his problem, help him identify the most appropriate technique(s), andgive him sufficient knowledge to interact with the appropriate analytical specialists, thereby enabling materials

characterization and troubleshooting to be conducted effectively and efficiently. The intent of this Handbook ismake an engineer a materials characterization specialist. not to

During the planning of this Handbook, it became obvious that the phrase "materials characterization" had to be carefullydefined in order to limit the scope of the book to a manageable size. Materials characterization represents many different

disciplines depending upon the background of the user. These concepts range from that of the scientist, who thinks of it inatomic terms, to that of the process engineer, who thinks of it in terms of properties, procedures, and quality assurance, to

that of the mechanical engineer, who thinks of it in terms of stress distributions and heat transfer. The definition selectedfor this book is adopted from that developed by the Committee on Characterization of Materials, Materials Advisory

Board, National Research Council (Ref 1): "Characterization describes those features of composition and structure(including defects) of a material that are significant for a particular preparation, study of properties, or use, and suffice for

reproduction of the material." This definition limits the characterization methods included herein to those that provideinformation about composition, structure, and defects and excludes those methods that yield information primarily related

to materials properties, such as thermal, electrical, and mechanical properties.

Most characterization techniques (as defined above) that are in general use in well-equipped materials analysislaboratories are described in this Handbook. These include methods used to characterize materials such as alloys, glasses,

ceramics, organics, gases, inorganics, and so on. Techniques used primarily for biological or medical analysis are notincluded. Some methods that are not widely used but that give unique or critical information are also described.

Techniques that are used primarily for highly specialized fundamental research or that yield information not consistentwith our definition of materials characterization have been omitted. Several techniques may be applicable for solving a

particular problem, providing the engineer, materials scientist, and/or analyst with a choice or with the possibility of usingcomplementary methods. With the exception of gas chromatography/mass spectroscopy, tandem methods that combine

two or more techniques are not discussed, and the reader is encouraged to refer to the descriptions of the individualmethods.

Reference

1. Characterization of Materials, Advisory Board, MAB-229-M, March 1967 prepared by The Committee on Characterization of Materials, Materials

Introduction to Materials Characterization R.E. Whan, Materials Characterization Department, Sandia National Laboratories

Organization

The Handbook has been organized for ease of reference by the user. The article "How To Use the Handbook" describesthe tables, flow charts, and extensive cross-referenced index that can be used to quickly identify techniques applicable to

a given problem. The article "Sampling" alerts the reader to the importance of sampling and describes proper methods forobtaining representative samples.

The largest subdivisions of the Handbook have been designated as Sections, each of which deals with a set of relatedtechniques, for example, "Electron Optical Methods." Within each Section are several articles, each describing a separate

analytical technique. For example, in the Section on "Electron Optical Methods" are articles on "Analytical TransmissionElectron Microscopy," "Scanning Electron Microscopy," "Electron Probe X-Ray Microanalysis," and "Low-Energy

Electron Diffraction." Each article begins with a summary of general uses, applications, limitations, sample requirements,and capabilities of related techniques, which is designed to give the reader a quick overview of the technique, and to help

him decide whether the technique might be applicable to his problem. This summary is followed by text that describes insimplified terms how the technique works, how the analyses are performed, what kinds of information can be obtained,

and what types of materials problems can be addressed. Included are several brief examples that illustrate how thetechnique has been used to solve typical problems. A list of references at the end of each article directs the reader to more

detailed information on the technique.

Following the last Section is a "Glossary of Terms" and appendices on metric conversion data and abbreviations,acronyms, and symbols used throughout the Volume. The Handbook concludes with a detailed cross-referenced index

that classifies the entries by technique names, types of information or analyses desired, and classes of materials. Thisindex, combined with the tables and flow charts in the article "How To Use the Handbook," is designed to enable the user

to quickly determine which techniques are most appropriate for his problem.

Introduction to Materials Characterization R.E. Whan, Materials Characterization Department, Sandia National Laboratories Reference

1. Characterization of Materials, Advisory Board, MAB-229-M, March 1967 prepared by The Committee on Characterization of Materials, Materials

How To Use the Handbook R.E. Whan, K.H. Eckelmeyer, and S.H. Weissman, Sandia National Laboratories

Effective Analytical Approach

The key to the successful solution of most materials problems is close interaction between the appropriate engineers,materials scientists, and analytical specialists. Engineers and other applications-oriented personnel are often the first to

encounter material failures or other problems. When this occurs, consultation with a materials specialist is an essentialfirst step in the troubleshooting process. By virtue of his knowledge of materials, the materials specialist can help the

engineer define the problem, identify possible causes, and determine what type of information (analytical or otherwise) isneeded to verify or refute each possible cause. Once a decision has been made regarding the information needed, they

must determine which analytical techniques appear most applicable to the problem.

With the large number of techniques available, it is often difficult to identify the best method or methods for a givenproblem. The goal of this Handbook is to help engineers and materials scientists identify the most applicable analytical

methods and interact effectively with the appropriate analytical specialists, who can help define the analytical test matrix,determine sampling procedures, take the data, and assist in interpreting the data. Together, these workers can solve

problems much more effectively than could be done by any one, or even any two, of them.

This collaborative approach to solving a problem has many benefits. When the analyst is fully informed about the natureof the problem and its possible causes, he is much more likely to understand what to look for and how best to look for it.

He may be able to suggest complementary or alternative techniques that will yield supplemental and/or more useful

Table 1 Inorganic solids: metals, alloys, semiconductors Wet analytical chemistry, electrochemistry, ultraviolet/visible absorption spectroscopy, and molecular fluorescence spectroscopy can generally be adapted to perform many of the bulk

analyses listed. • = generally usable; N orspecial conditions; D = after dissolution; Z or ** = semiconductors only = limited number of elements or groups; G = carbon, nitrogen, hydrogen, sulfur, or oxygen: see summary in article for details; S or * = under

Method Elem Alloy ver Iso/Mass Qual Semiquant Quant Macro/Bulk Micro Surface Major Minor Trace Phase ID Structure Morphology AAS D D D D D D AES • • • • • • • S S COMB G G G G G G EPMA • S • • • • • • N S • ESR N N N N N N N N IA • • • IC D, N D, N D, N D, N D, N D, N D, N D, N ICP-AES D D D D D D D D D IGF G G G G G G IR/FT-IR Z Z Z Z Z Z Z LEISS • • • S • • • • NAA • N • • • • • •

OES • • • • • • • • •

OM • • •

RBS • • • • • • S S

RS Z Z Z Z Z Z Z Z

SEM • • • S • • • S •

SIMS • • • • • • S

SSMS • • • • • • • • • •

TEM • • • S • • • • • •

XPS • • • • • •

XRD • • S • • • • •

XRS • • • • • • • • N

Abbreviations in the column headings are defined in Table 9. The method acronyms are defined in Table 10.

RS S S S S S S S S S S S

SEM • • • • • • S •

SIMS • • • • • • S

SSMS • • • • • • • • •

TEM • • • S • • • • • •

XPS • N • • • • •

XRD • • • S • • • • •

XRS • • • • • • • N

Abbreviations in the column headings are defined in Table 9. The method acronyms are defined in Table 10.

NAA • N • • • • • • •

OES • • • • • • • •

OM • • •

RBS • • • • • • • S S

RS S, D S, D S, D S, D S, D S S, D S, D S, D S, D S, D

SEM • • • • • • S •

SIMS • • • • • • S S

SSMS • • • • • • • • •

TEM • • • S • • • • • •

XPS • • • • • • • S

XRD • • S • • • • •

XRS • • • • • • • N

Abbreviations in the column headings are defined in Table 9. The method acronyms are defined in Table 10.

Table 4 Inorganic liquids and solutions: water, effluents, leachates, acids, bases, chemical reagents Wet analytical chemistry, electrochemistry, ultraviolet/visible absorption spectroscopy, and molecular fluorescence spectroscopy can generally be adapted to perform the bulk analyses

listed. Most of techniques listed for inorganic solids can be used on the residue after the solution is evaporated to dryness. • = generally usable; N orgroups; S = under special conditions; V or * = volatile liquids or components = limited number of elements or

Method Elem Speciation Compound Iso/Mass Qual Semiquant Quant Macro/Bulk Major Minor Trace Structure AAS • • • • • • EFG N N N N N N N N N ESR N N N N N N N N N GC/MS V, N V V V V V V V V GMS V, N V V V V V V V V V IC • • S • • • • • • • ICP-AES • • • • • • • • IR/FT-IR • • • • • • • • • • ISE • S • • • • • • NAA • N • • • • • • • NMR N N N N N N N RS • • • • • • • • S