springer handbook of materials measurement...
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Springer Handbookof Materials Measurement Methods
Springer Handbooks providea concise compilation of approvedkey information on methods ofresearch, general principles, andfunctional relationships in physi-cal sciences and engineering. Theworld’s leading experts in the fieldsof physics and engineering will beassigned by one or several renownededitors to write the chapters com-prising each volume. The contentis selected by these experts fromSpringer sources (books, journals,online content) and other systematicand approved recent publications ofphysical and technical information.
The volumes will be designed tobe useful as readable desk referencebooks to give a fast and comprehen-sive overview and easy retrieval ofessential reliable key information,including tables, graphs, and bibli-ographies. References to extensivesources are provided.
123
HandbookSpringerof Materials Measurement
MethodsHorst Czichos, Tetsuya Saito, Leslie Smith (Eds.)
With CD-ROM, 970 Figures and 158 Tables
Editors:Horst CzichosFederal Institute for Materials Researchand Testing (BAM), Past President;University of Applied Sciences BerlinGermany
Tetsuya SaitoNational Institute for Materials Science (NIMS)Tsukuba, IbarakiJapan
Leslie SmithNational Institute of Standards and Technology (NIST)Gaithersburg, MDUSA
Library of Congress Control Number: 2006921595
ISBN-10: 3-540-20785-6 e-ISBN: 3-540-30300-6ISBN-13: 978-3-540-20785-6 Printed on acid free paper
c© 2006, Springer Science+Business Media, Inc.This work is subject to copyright. All rights reserved, whether the wholeor part of the material is concerned, specifically the rights of translation,reprinting, reuse of illustrations, recitation, broadcasting, reproduction onmicrofilm or in any other way, and storage in data banks. Duplication ofthis publication or parts thereof is permitted only under the provisions ofthe German Copyright Law of September, 9, 1965, in its current version,and permission for use must always be obtained from Springer-Verlag.Violations are liable for prosecution under the German Copyright Law.
The use of designations, trademarks, etc. in this publication does not imply,even in the absence of a specific statement, that such names are exempt fromthe relevant protective laws and regulations and therefore free for generaluse.
Product liability: The publisher cannot guarantee the accuracy of anyinformation about dosage and application contained in this book. In everyindividual case the user must check such information by consulting therelevant literature.
Production and typesetting: LE-TeX GbR, LeipzigHandbook coordinator: Dr. W. Skolaut, HeidelbergTypography, layout and illustrations:schreiberVIS, Seeheim & Hippmann GbR, SchwarzenbruckCover design: eStudio Calamar Steinen, BarcelonaCover production: WMXDesign GmbH, HeidelbergPrinting and binding: Stürtz AG, Würzburg
SPIN 10918104 62/3141/YL 5 4 3 2 1 0
V
Preface
The ability to compare measurements between labora-tories is one of the cornerstones of the scientific method.All scientists and engineers are trained to make accu-rate measurements and a comprehensive volume thatprovides detailed advice and leading references on meas-urements to scientific and engineering professionalsand students is always a worthwhile addition to theliterature. The principal motivation for this SpringerHandbook of Materials Measurement Methods, how-ever, stems from the increasing demands of technologyfor measurement results that can be used reliably any-where in the world. These demands are especiallyintense in materials science and technology, where manycharacterization methods are needed, from scientificcomposition–structure–property relations to techno-logical performance–quality–reliability assessmentdata, during the various stages of materials and productcycles.
In order for new materials to be used and incor-porated into practical technology, their most importantcharacteristics must be known well enough to justifylarge research and development costs. Furthermore, theresearch may be performed in one country while theengineering design is done in another and the proto-type manufacture in yet another region of the world.This great emphasis on international comparison meansthat increasing attention must be paid to internation-ally recognized standards and calibration methods thatgo beyond careful, internally consistent, methods. Thishandbook was developed to assist scientists and en-gineers in both industry and academe in this task.
The useful properties of materials are generally re-sponses to external fields under specific conditions. Thestimulus field and environmental conditions must becompletely specified in order to develop a reproducibleresponse. Standard test methods describe these condi-tions and the Chapters and an Appendix in this book con-tain references to the relevant international standards.
Horst Czichos
Tetsuya Saito
Leslie Smith
We sought out experts fromall over the world that have beeninvolved with concerns such asthese. We were extremely fortunateto find a distinguished set of au-thors who met the challenge: towrite brief chapters that nonethelesscontain specific useful recommen-dations and resources for furtherinformation. This is the hallmark ofa successful handbook. While the di-verse nature of the topics coveredhas led to different styles of pre-sentation, there is a commonality ofpurpose evident in the chapters thatcome from the authors’ understand-ing of the issues facing researcherstoday.
This handbook would not havebeen possible without the vision-ary support of Dr. Hubertus vonRiedesel, who embraced the con-cept and encouraged us to pursueit. We must also acknowledge theconstant support of Dr. Werner Sko-laut, whose technical editing has metevery expectation of professionalexcellence. Finally, throughout theentire development of the handbookwe were greatly aided by the able ad-ministrative support of Ms. DanielaBleienberger.
March 2006Horst Czichos, Tetsuya Saito,Leslie Smith (Editors)Berlin/Tsukuba/Washington
VII
List of Authors
Shuji AiharaNippon Steel CorporationSteel Research Laboratories20-1, Shintomi FuttsuChiba, 293-8511, Japane-mail: [email protected]
Tsutomu ArakiOsaka UniversityGraduate School of Engineering ScienceMachikaneyama, ToyonakaOsaka, 560-8531, Japane-mail: [email protected]
Masaaki AshidaOsaka UniversityGraduate School of Engineering Science1-3 Machikaneyama-cho, ToyonakaOsaka, 560-8531, Japane-mail: [email protected]
Peter D. AskewIMSL, Industrial Microbiological Services LimitedPale LaneHartley Wintney, Hants RG27 8DH, UKe-mail: [email protected]
Heinz-Gunter BachHeinrich-Hertz-InstitutComponents/Integration Technology,Fraunhofer-Institute for TelecommunicationsEinsteinufer 3710587 Berlin, Germanye-mail: [email protected]
Gun-Woong BahngKorea Research Institute of Standards and ScienceDivision of Chemical and Materials MetrologyDoryong-dong 1, POBox 102, YuseoungDaejeon, 305-600, South Koreae-mail: [email protected]
Claude BathiasConservatoire National des Arts et Métiers,Laboratoire ITMAInstitute of Technology and Advanced Materials2 rue Conté75003 Paris, Francee-mail: [email protected]
Günther BayreutherUniversity of RegensburgPhysics DepartmentUniversitätsstr. 3193040 Regensburg, Germanye-mail:[email protected]
Nick BoleyLGC Ltd.Proficiency Testing and TrainingQueens RoadTeddington, TW11 0LY, UKe-mail: [email protected]
Wolfgang BuckPhysikalisch-Technische Bundesanstalt,Institut BerlinDivision 7Abbestrasse 2–1210587 Berlin, Germanye-mail: [email protected]
Richard R. CavanaghNational Institute of Standardsand Technology (NIST)Surface and Microanalysis Science Division,Chemical Science and Technology Laboratory (CSTL)100 Bureau Drive, MS 8371Gaithersburg, MD 20899, USAe-mail: [email protected]
VIII List of Authors
Leonardo De ChiffreTechnical University of DenmarkDepartment of Manufacturing Engineeringand ManagementProduktionstorvet, Building 425Kgs. Lyngby, 2800, Denmarke-mail: [email protected]
Steven J. ChoquetteNational Institute of Standards and TechnologyBiochemical Science Division100 Bureau Dr., MS 8312Gaithersburg, MD 20899-8312, USAe-mail: [email protected]
Horst CzichosUniversity of Applied Sciences BerlinDepartment of Electrical Engineeringand Precision EngineeringTFH Berlin, Luxemburger Strasse 1013353 Berlin, Germanye-mail: [email protected]
Werner DaumFederal Institute for Materials Researchand Testing (BAM)Division VIII.1Unter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Paul DeRoseNational Institute of Standards and TechnologyBiochemical Science Division100 Bureau Drive, MS 8312Gaithersburg, MD 20899-8312, USAe-mail: [email protected]
Stephen L.R. EllisonLGC Ltd.Bioinformatics and StatisticsQueens Road, TeddingtonMiddlesex, TW11 0LY, UKe-mail: [email protected]
Anton ErhardFederal Institute for Materials Researchand Testing (BAM)Department Non-destructive Testing; Acousticaland Electrical MethodsUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Uwe EwertFederal Institute for Materials Researchand Testing (BAM)Division VIII.3 RadiologyUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Richard J. FieldsNational Institute of Standards and TechnologyMaterials Science and Engineering Laboratory100 Bureau DriveGaithersburg, MD 20899, USAe-mail: [email protected]
Benny D. FreemanThe University of Texas at Austin, Center for Energyand Environmental ResourcesDepartment of Chemical Engineering10100 Burnet Road, Building 133, R-7100Austin, TX 78758, USAe-mail: [email protected]
Mark GeeNational Physical LaboratoryDivision of Engineering and Processing ControlHampton RoadTeddington, TW11 0LW , UKe-mail: [email protected]
Jürgen GoebbelsFederal Institute for Materials Researchand Testing (BAM)Radiology (VIII.3)Unter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
List of Authors IX
Anna A. GorbushinaCarl von Ossietzky Universität OldenburgGeomicrobiology, ICBM26111 Oldenburg, Germanye-mail: [email protected]
Robert R. GreenbergNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Drive, MS 8395Gaithersburg, MD 20899-8395, USAe-mail: [email protected]
Manfred GrindaLandreiterweg 2212353 Berlin, Germanye-mail: [email protected]
Roland GrössingerTechnical University ViennaInstitut für FestkörperphysikWiedner Hauptstr. 8–10Vienna, Austriae-mail: [email protected]
Yukito HagiharaSophia UniversityFaculty of Science and Technology, Department ofMechanical Engineering7–1 Kioi-cho, Chiyoda-kuTokyo, 102-8554, Japane-mail: [email protected]
Junhee HahnKorea Research Institute of Standardsand Science (KRISS)Chemical Metrology and Materials Evaluation Div.Yuseong, 102Daejeon, 305-622, South Koreae-mail: [email protected]
Holger HanselkaFraunhofer-Institute for Structural Durability andSystem Reliability (LBF)Bartningstrasse 4764289 Darmstadt, Germanye-mail: [email protected]
Manfred P. HentschelFederal Institute for Materials Researchand Testing (BAM)VIII.3, Nondestructive Testing12200 Berlin, Germanye-mail: [email protected]
Horst HertelFederal Institute for Materials Researchand Testing (BAM)Division IV.1Unter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Ian HutchingsUniversity of Cambridge,Institute for ManufacturingDepartment of EngineeringMill LaneCambridge, CB2 1RX, UKe-mail: [email protected]
Xiao HuNational Institute for Materials ScienceStrong Coupling Modeling Group, ComputationalMaterials Science CenterSengen 1-2-1Tsukuba, 305-0047, Japane-mail: [email protected]
Werner HässelbarthFederal Institute for Materials Researchand Testing (BAM)Analytical Chemistry; Reference MaterialsRichard-Willstätter-Str. 1112489 Berlin, Germanye-mail: [email protected]
Shoji ImataniKyoto UniversityDepartment of Energy Conversion ScienceYoshida-honmachi, Sakyo-kuKyoto, 606-8501, Japane-mail: [email protected]
X List of Authors
Hanspeter IschiThe Swiss Accreditation Service (SAS)Lindenweg 50Berne, CH 3003, Switzerlande-mail: [email protected]
Bernd IseckeFederal Institute for Materials Researchand Testing (BAM)Corrosion and Corrosion ProtectionUnter den Eichen 8712203 Berlin, Germanye-mail: [email protected]
Tadashi ItohGraduate School of Engineering Science,Osaka UniversityDepartment of Materials Engineering Science1-3, Machikaneyama-cho, ToyonakaOsaka, 560-8531, Japane-mail: [email protected]
Tetsuo IwataThe University of TokushimaDepartment of Mechanical Engineering2-1, Minami-JyosanjimaTokushima, 770-8506, Japane-mail: [email protected]
Gerd-Rüdiger JaenischFederal Institute for Materials Researchand Testing (BAM)Non-destructive TestingUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Oliver JannFederal Institute for Materials Researchand Testing (BAM)Emissions from MaterialsUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Masanori KohnoNational Institute for Materials ScienceComputational Materials Science Center1-2-1 SengenTsukuba, 305-0047, Japane-mail: [email protected]
Toshiyuki KoyamaNational Institute for Materials ScienceComputational Materials Science Center1-2-1 Sengen, TsukubaIbaraki, 305-0047, Japane-mail: [email protected]
Gary W. KramerNational Institute of Standards and TechnologyBiospectroscopy Group, Biochemical ScienceDivision100 Bureau DriveGaithersburg, MD 20899-8312, USAe-mail: [email protected]
Wolfgang E. KrumbeinBIOGEMAMaterial EcologyLindenweg 16a26188 Edewecht, Germanye-mail: [email protected]
George LamazeNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Dr. Stop 8395Gaithersburg, MD 20899, USAe-mail: [email protected]
Richard LindstromNational Institute of Standards and Technology,Mail stop 8395Analytical Chemistry DivisionGaithersburg, MD 20899-8395, USAe-mail: [email protected]
Haiqing LinMembrane Technology and Research, Inc.1306 Willow Road, Suite 103Menlo Park, CA 94025, USAe-mail: [email protected]
List of Authors XI
Samuel LowNational Institute of Standards and TechnologyMetallurgy Division, Materials Scienceand Engineering Laboratory100 Bureau Drive, Mail Stop 8553Gaithersburg, MD 20899, USAe-mail: [email protected]
Koji MaedaThe University of TokyoDepartment of Applied PhysicsHongo, Bunkyo-kuTokyo, 113-8656, Japane-mail: [email protected]
Willie E. MayNational Institute of Standardsand Technology (NIST)Chemical Science and Technology Laboratory (CSTL)100 Bureau Drive, MS 8300Gaithersburg, MD 20899, USAe-mail: [email protected]
Takashi MiyataNagoya UniversityDepartment of Materials Science and EngineeringNagoya, 464-8603, Japane-mail: [email protected]
Hiroshi MizubayashiUniversity of TsukubaInstitute of Materials ScienceTsukuba, Ibaraki 305-8573, Japane-mail: [email protected]
Kiyofumi MuroChiba UniversityFaculty of Science, Department of Physics1-33 Yayoi-cho, Inage-kuChiba, 283-8522, Japane-mail: [email protected]
Rolf-Joachim MüllerGesellschaft für Biotechnologische Forschung mbHTU-BCEMascheroder Weg 138124 Braunschweig, Germanye-mail: [email protected]
Yoshihiko NonomuraNational Institute for Materials ScienceComputational Materials Science CenterSengen 1-2-1, TsukubaIbaraki, 305-0047, Japane-mail: [email protected]
Jürgen NufferFraunhofer Institute for Structural Durability andSystem Reliability (LBF)Bartningstrasse 4764289 Darmstadt, Germanye-mail: [email protected]
Jan ObrzutNational Institute of Standards and TechnologyPolymers Division100 Bureau Dr.Gaithersburg, MD 20899-8541, USAe-mail: [email protected]
Hiroshi OhtaniKyushu Institute of TechnologyDepartment of Materials Science and EngineeringSensui-cho 1-1, Tobata-kuKitakyushu, 804-8550, Japane-mail: [email protected]
Kurt OsterlohFederal Institute for Materials Researchand Testing (BAM)Division VIII.3Unter den Eichen 9712205 Berlin, Germanye-mail: [email protected]
Michael PantkeFederal Institute for Materials Researchand Testing (BAM)Division IV.1, Materials and Environment12205 Berlin, Germanye-mail: [email protected]
XII List of Authors
Karen W. PhinneyNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Drive, Stop 8392Gaithersburg, MD 20899-8392, USAe-mail: [email protected]
Rüdiger (Rudy) PlarreFederal Institute for Materials Researchand Testing (BAM)Environmental Compatibility of MaterialsUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Kenneth W. PrattNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Dr., Stop 8391Gaithersburg, MD 20899-8391, USAe-mail: [email protected]
Michael H. RamseyUniversity of SussexDepartment of Biology and EnvironmentalScience, Centre for Environmental ResearchSussex HouseBrighton, BN1 9RH, UKe-mail: [email protected]
Gunnar RossMagnet-Physik Dr. Steingroever GmbHEmil-Hoffmann-Str. 350996 Köln, Germanye-mail: [email protected]
Steffen RudtschPhysikalisch-Technische Bundesanstalt (PTB)Dept. 7.4Abbestr. 2–1210587 Berlin, Germanye-mail: [email protected]
Lane SanderNational Institute of Standards and TechnologyChemical Science and Technology Laboratory,Analytical Chemistry Division100 Bureau Drive, MS 8392Gaithersburg, MD 20899-8392, USAe-mail: [email protected]
Erich SantnerFederal Institute for Materials Researchand Testing (BAM)Unter den Eichen 44–4612203 Berlin, Germanye-mail: [email protected]
Michele SchantzNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Drive, Stop 8392Gaithersburg, MD 20899, USAe-mail: [email protected]
Guenter SchmittIserlohn University of Applied SciencesLaboratory for Corrosion ProtectionFrauenstuhlweg 318644 Iserlohn, Germanye-mail: [email protected]
Bernd SchumacherPhysikalisch-Technische BundesanstaltDepartment 2.1 DC and Low FrequencyBundesallee 10038116 Braunschweig, Germanye-mail: [email protected]
Karin SchwibbertFederal Institute for Materials Researchand Testing (BAM)Division IV.1 Materials and Environment12205 Berlin, Germanye-mail: [email protected]
List of Authors XIII
Michael SchützeKarl-Winnacker-InstitutDECHEMA e.V.Theodor-Heuss-Allee 2560486 Frankfurt am Main, Germanye-mail: [email protected]
John Henry ScottNational Institute of Standards and TechnologySurface and Microanalysis Science Division100 Bureau Drive, MS 8370Gaithersburg, MD 20899, USAe-mail: [email protected]
Martin SeahNational Physical LaboratoryQuality of Life DivisionHampton Road, MiddlesexTeddington, TW11 0LW, UKe-mail: [email protected]
Masato ShimonoNational Institute for Materials ScienceComputational Materials Science Center1-2-1 SengenTsukuba, 305-0047, Japane-mail: [email protected]
John R. SieberNational Institute of Standards and TechnologyChemical Science and Technology Laboratory100 Bureau Drive, Stop 8391Gaithersburg, MD 20899, USAe-mail: [email protected]
Franz-Georg SimonFederal Institute for Materials Researchand Testing (BAM)Waste Treatment and Remedial EngineeringUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
John SmallNational Institute of Standards and TechnologySurface and Microanalysis Science Division100 Bureau Drive, MS 8370Gaithersburg, MD 20899, USAe-mail: [email protected]
Melody V. SmithNational Institute of Standards and TechnologyPhysical Science Technician (WEG), BiospectroscopyGroup, Biochemical Science Division100 Bureau DriveGaithersburg, MD 20899-8312, USAe-mail: [email protected]
Petra SpitzerPhysikalisch-Technische Bundesanstalt (PTB)Dept. 3.13 Metrology in ChemistryBundesallee 10038116 Braunschweig, Germanye-mail: [email protected]
Ina StephanFederal Institute for Materials Researchand Testing (BAM)Division IV.1 Biology in Materials Protectionand Environmental IssuesUnter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Stephan J. StranickNational Institute of Standards and TechnologyDepartment of Commerce, Surfaceand Microanalysis Science Division100 Bureau Dr. Stop 8372Gaithersburg, MD 20899-8372, USAe-mail: [email protected]
Hans-Henning StrehblowHeinrich-Heine-UniversitätInstitute of Physical ChemistryUniversitätsstr. 140225 Düsseldorf, Germanye-mail: [email protected]
XIV List of Authors
Tetsuya TagawaNagoya UniversityDepartment of Materials Science and EngineeringNagoya, 464-8603, Japane-mail: [email protected]
Akira TezukaNational Institute of Advanced Industrial Scienceand TechnologyAdvanced Manufacturing Research InstituteAIST Tsukuba EastTsukuba, 305-8564, Japane-mail: [email protected]
Yo TomotaIbaraki UniversityDepartment of Materials Science,Faculty of Engineering4-12-1 Nakanarusawa-choHitachi, 316-8511, Japane-mail: [email protected]
John TravisNational Institute of Standards and TechnologyAnalytical Chemistry Division (Retired)100 Bureau Drive, MS 8312Gaithersburg, MD 20899-8312, USAe-mail: [email protected]
Gregory C. TurkNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Drive, Stop 8391Gaithersburg, MD 20899, USAe-mail: [email protected]
Thomas VetterNational Institute of Standardsand Technology (NIST)Analytical Chemistry Division100 Bureau Dr. Stop 8391Gaithersburg, MD 20899-8391, USAe-mail: [email protected]
Andrew WallardPavillon de BreteuilBureau International des Poids Et Mesures92312 Sèvres, Francee-mail: [email protected]
Joachim WeckerSiemens AGCorporate TechnologyP.O.Box 322091050 Erlangen, Germanye-mail: [email protected]
Wolfhard WegscheiderMontanuniversität LeobenGeneral and Analytical ChemistryFranz-Josef-Strasse 18Leoben, 8700, Austriae-mail: [email protected]
Alois WehrstedtDIN Deutsches Institut für NormungNormenausschuss Materialprüfung (NMP)Burggrafenstraße 610787 Berlin, Germanye-mail: [email protected]
Michael WelchNational Institute of Standards and Technology100 Bureau Drive, Stop 8392Gaithersburg, MD 20899, USAe-mail: [email protected]
Ulf WickströmSP Swedish National Testing and Research InstituteDepartment of Fire TechnologyP.O. Box 857SE-501 15 Borås, Swedene-mail: [email protected]
Sheldon M. WiederhornNational Institute of Standards and TechnologyMaterials Science and Engineering Laboratory100 Bureau DriveGaithersburg, MD 20899-8500, USAe-mail: [email protected]
List of Authors XV
Scott WightNational Insitute of Standards and TechnologySurface and Microanalysis Science Division100 Bureau Drive, Stop 8371Gaithersburg, MD 20899-8371, USAe-mail: [email protected]
Michael WinchesterNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Drive, Building 227, Mailstop 8391Gaithersburg, MD 20899, USAe-mail: [email protected]
Noboru YamadaMatsushita Electric Industrial Company, Ltd.Optical Media Group, Storage Media SysytemsDevelopment Center3-1-1 Yagumo-NakamachiMoriguchi, 570-8501, Japane-mail: [email protected]
Rolf ZeislerNational Institute of Standards and TechnologyAnalytical Chemistry Division100 Bureau Drive, MS 8395Gaithersburg, MD 20899-8395, USAe-mail: [email protected]
Uwe ZscherpelFederal Institute for Materials Researchand Testing (BAM)Division “NDT – Radiological Methods”Unter den Eichen 8712205 Berlin, Germanye-mail: [email protected]
Adolf ZschunkeRapsweg 11504207 Leipzig, Germanye-mail: [email protected]
XVII
Contents
List of Abbreviations ................................................................................. XXIII
Part A Materials Measurement System
1 Measurement Principles and Structures............................................. 31.1 What Is Metrology? ........................................................................ 31.2 The Roots and Evolution of Metrology............................................. 31.3 BIPM: The Birth of the Meter Convention ........................................ 61.4 BIPM: The First 75 Years ................................................................. 71.5 Quantum Standards: A Metrological Revolution............................... 81.6 Regional Metrology Organizations .................................................. 91.7 Traceability of Measurements......................................................... 101.8 Mutual Recognition of NMI Standards: The CIPM MRA....................... 101.9 Metrology in the 21st Century ......................................................... 121.10 The SI System and New Science ...................................................... 14References............................................................................................... 16
2 Measurement Strategy and Quality .................................................... 172.1 Sampling ...................................................................................... 182.2 The Traceability of Measurements .................................................. 232.3 Statistical Evaluation of Results ...................................................... 272.4 Validation ..................................................................................... 472.5 Inter-laboratory Comparisons and Proficiency Testing ..................... 572.6 (Certified) Reference Materials ....................................................... 672.7 Reference Procedures .................................................................... 752.8 Accreditation and Peer Assessment ................................................ 842.9 Human Aspects in a Laboratory ...................................................... 882.10 Further Reading ............................................................................ 92References............................................................................................... 92
3 Materials and Their Characteristics: Overview ................................... 953.1 Basic Features of Materials ............................................................ 963.2 Classification of Materials Characterization Methods ....................... 101References............................................................................................... 102
Part B Measurement Methods for Compositionand Structure
4 Chemical Composition.......................................................................... 1054.1 Bulk Chemical Characterization ...................................................... 1054.2 Microanalytical Chemical Characterization ...................................... 138References............................................................................................... 148
XVIII Contents
5 Nanoscopic Architecture and Microstructure ..................................... 1535.1 Fundamentals ............................................................................... 1595.2 Crystalline and Amorphous Structure Analysis ................................. 1805.3 Lattice Defects and Impurities Analysis ........................................... 1875.4 Molecular Architecture Analysis ...................................................... 2065.5 Texture, Phase Distributions, and Finite Structures Analysis ............. 217References............................................................................................... 225
6 Surface and Interface Characterization .............................................. 2296.1 Surface Chemical Analysis .............................................................. 2306.2 Surface Topography Analysis .......................................................... 255References............................................................................................... 272
Part C Measurement Methods for Materials Properties
7 Mechanical Properties ......................................................................... 2837.1 Elasticity ....................................................................................... 2847.2 Plasticity ....................................................................................... 2997.3 Hardness ...................................................................................... 3117.4 Strength ....................................................................................... 3337.5 Fracture Mechanics ........................................................................ 3537.6 Permeation and Diffusion .............................................................. 371References............................................................................................... 387
8 Thermal Properties............................................................................... 3998.1 Thermal Conductivity and Specific Heat Capacity ............................. 4008.2 Enthalpy of Phase Transition, Adsorption and Mixing ...................... 4088.3 Thermal Expansion and Thermomechanical Analysis ....................... 4158.4 Thermogravimetry ......................................................................... 4178.5 Temperature Sensors ..................................................................... 417References............................................................................................... 428
9 Electrical Properties ............................................................................. 4319.1 Electrical Materials ........................................................................ 4329.2 Electrical Conductivity of Metallic Materials..................................... 4399.3 Electrolytical Conductivity .............................................................. 4449.4 Semiconductors ............................................................................. 4539.5 Measurement of Dielectric Materials Properties ............................... 472References............................................................................................... 481
10 Magnetic Properties ............................................................................. 48510.1 Magnetic Materials ........................................................................ 48610.2 Soft and Hard Magnetic Materials: (Standard) Measurement
Techniques for Properties Related to the B(H) Loop ......................... 49010.3 Magnetic Characterization in a Pulsed Field Magnetometer (PFM) .... 51010.4 Properties of Magnetic Thin Films ................................................... 522References............................................................................................... 527
Contents XIX
11 Optical Properties ................................................................................. 53111.1 Fundamentals of Optical Spectroscopy ............................................ 53211.2 Micro-spectroscopy ....................................................................... 54911.3 Magnetooptical Measurement ........................................................ 55311.4 Nonlinear Optics and Ultrashort Pulsed Laser Application ................ 55811.5 Fiber Optics ................................................................................... 57011.6 Evaluation Technologies for Optical Disk Memory Materials .............. 58511.7 Optical Sensing ............................................................................. 593References............................................................................................... 600
Part D Measurement Methods for Materials Performance
12 Corrosion ............................................................................................... 61112.1 Background .................................................................................. 61212.2 Conventional Electrochemical Test Methods .................................... 61512.3 Novel Electrochemical Test Methods ............................................... 63912.4 Exposure and On-Site Testing ........................................................ 64312.5 Corrosion Without Mechanical Loading ........................................... 64312.6 Corrosion with Mechanical Loading ................................................ 64912.7 Hydrogen-Induced Stress Corrosion Cracking .................................. 65912.8 High-Temperature Corrosion .......................................................... 66212.9 Inhibitor Testing and Monitoring of Efficiency................................. 676References............................................................................................... 681
13 Friction and Wear................................................................................. 68513.1 Definitions and Units..................................................................... 68513.2 Selection of Friction and Wear Tests ............................................... 68913.3 Tribological Test Methods ............................................................... 69313.4 Friction Measurement .................................................................... 69613.5 Quantitative Assessment of Wear ................................................... 70113.6 Characterization of Surfaces and Debris .......................................... 706References............................................................................................... 709
14 Biogenic Impact on Materials ............................................................. 71114.1 Modes of Materials – Organisms Interactions .................................. 71214.2 Biological Testing of Wood ............................................................. 71614.3 Testing of Organic Materials ........................................................... 73114.4 Biological Testing of Inorganic Materials ......................................... 75314.5 Coatings and Coating Materials ...................................................... 76814.6 Reference Organisms ..................................................................... 775References............................................................................................... 780
15 Material–Environment Interactions ................................................... 78915.1 Materials and the Environment ...................................................... 78915.2 Emissions from Materials ............................................................... 80415.3 Fire Physics and Chemistry ............................................................. 813References............................................................................................... 825
XX Contents
16 Performance Control and Condition Monitoring ............................... 83116.1 Nondestructive Evaluation ............................................................. 83216.2 Industrial Radiology ...................................................................... 84416.3 Computerized Tomography – Application to Organic Materials ......... 85816.4 Computerized Tomography – Application to Inorganic Materials ...... 86416.5 Computed Tomography – Application to Composites
and Microstructures ....................................................................... 87016.6 Structural Health Monitoring – Embedded Sensors.......................... 87516.7 Characterization of Reliability ........................................................ 89116.A Appendix ...................................................................................... 907References............................................................................................... 908
Part E Modeling and Simulation Methods
17 Molecular Dynamics ............................................................................. 91517.1 Basic Idea of Molecular Dynamics ................................................... 91517.2 Diffusionless Transformation .......................................................... 92817.3 Rapid Solidification ....................................................................... 93517.4 Diffusion ....................................................................................... 94617.5 Summary ...................................................................................... 950References............................................................................................... 950
18 Continuum Constitutive Modeling ...................................................... 95318.1 Phenomenological Viscoplasticity ................................................... 95318.2 Material Anisotropy ....................................................................... 95818.3 Metallothermomechanical Coupling ............................................... 96318.4 Crystal Plasticity ............................................................................ 966References............................................................................................... 970
19 Finite Element and Finite Difference Methods .................................. 97319.1 Discretized Numerical Schemes for FEM and FDM ............................. 97519.2 Basic Derivations in FEM and FDM .................................................. 97719.3 The Equivalence of FEM and FDM Methods ...................................... 98119.4 From Mechanics to Mathematics: Equilibrium Equations
and Partial Differential Equations .................................................. 98219.5 From Mathematics to Mechanics:
Characteristic of Partial Differential Equations ................................ 98719.6 Time Integration for Unsteady Problems ......................................... 98919.7 Multidimensional Case .................................................................. 99119.8 Treatment of the Nonlinear Case .................................................... 99519.9 Advanced Topics in FEM and FDM ................................................... 99519.10 Free Codes .................................................................................... 999References............................................................................................... 999
Contents XXI
20 The CALPHAD Method............................................................................ 100120.1 Outline of the CALPHAD Method ...................................................... 100220.2 Incorporation of the First Principle Calculations
into the CALPHAD Approach ............................................................ 100620.3 Prediction of Thermodynamic Properties of Compound Phases
with First Principle Calculations ..................................................... 1019References............................................................................................... 1030
21 Phase Field ........................................................................................... 103121.1 Basic Concept of the Phase-Field Method ....................................... 103221.2 Total Free Energy of Microstructure ................................................. 103321.3 Solidification ................................................................................ 104221.4 Diffusion-Controlled Phase Transformation .................................... 104521.5 Structural Phase Transformation .................................................... 104821.6 Microstructure Evolution ................................................................ 1050References............................................................................................... 1054
22 Monte Carlo Simulation ....................................................................... 105722.1 Fundamentals of the Monte Carlo Method ...................................... 105722.2 Improved Algorithms ..................................................................... 106122.3 Quantum Monte Carlo Method ....................................................... 106622.4 Bicritical Phenomena in O(5) Model ................................................ 107322.5 Superconductivity Vortex State ....................................................... 107722.6 Effects of Randomness in Vortex States ........................................... 108322.7 Quantum Critical Phenomena......................................................... 1086References............................................................................................... 1089
Appendix – International Standards ....................................................... 1097Acknowledgements ................................................................................... 1151About the Authors ..................................................................................... 1153Detailed Contents ...................................................................................... 1173Subject Index ............................................................................................. 1189
XXIII
List of Abbreviations
μTA microthermal analysis
A
AA arithmetic averageAED atomic emission detectorAES Auger electron spectroscopyAFM atomic force microscopyAFNOR Association Française
de NormalisationAGM alternating gradient field magnetometerANOVA analysis of varianceAPCI atmospheric pressure chemical
ionizationAPD avalanche photodiodeARDRA amplified Ribosomal DNA Restriction
AnalysisASE amplified spontaneous emissionASTM American Society for Testing
and MaterialsATR attenuated total reflection
B
BAM Bundesanstalt für Materialforschungund -prüfung
BB Ladyzhenskaya–Babuska–Brezzicondition
BBB Ladyzhenskaya–Babuska–Brezzicondition
bcc body-centered cubicBEM Boundary Element MethodBLRF bispectral luminescence radiance factorBi-CGSTAB biconjugate gradient stabilized method
C
CAD computer-aided designCALPHAD calculation of phase diagramsCCD digitized with charge-coupled devicec.c.t. crevice corrosion temperatureCCT center-cracked tensionCE capillary electrophoresisCE counter electrodeCEM cluster expansion methodCEN European Standardisation OrganisationCERT constant extension rate testsCFD computational fluid dynamicsCFL Courant–Friedrichs–Lewy conditionCG conjugate gradient method
CIEF capillary isoelectric focusingCIP constrained interpolated profile methodCIPM International Committee for Weights
and MeasuresCITP capillary isotachophoresisCL cathodoluminescenceCLA center line averageCMA cylindrical mirror analyzerCMC calibration and measurement capabilityCPAA charged particle activation analysisc.p.t. critical pitting temperatureCRM certified reference materialCT compact tensionCTD charge transfer deviceCTE coefficient of thermal expansionCTS collaborative trial in samplingCVM cluster variation methodCW continuous waveCZE capillary zone electrophoresis
D
DA differential amplifierDC direct-currentDEM discrete element methodDFG difference-frequency generationDFT discrete Fourier transformDFT density functional theoryDIN Deutsches Institut für NormungDIR digital industrial radiologyDLTS deep level transient spectroscopyDOC dissolved organic carbonDOS density of statesDSC differential scanning calorimetry
E
EAM embedded-atom methodEBIC electron beam induced currentsECD electron capture detectorEDS energy-dispersive spectrometerEELS electron energy-loss spectroscopyEF emission factorsEHL elastohydrodynamically lubricatedEL electroluminescenceELSD evaporative light scattering detectorEMD easy magnetization directionEPMA electron probe microanalysisEPS extracellular polymeric substancesER emission rates
XXIV List of Abbreviations
ESEM environmental scanning electronmicroscope
ETS environmental tobacco smoke
F
fcc face-centered cubicFD finite differencesFDA frequency domain analysisFDM finite difference methodsFE finite elementsFEA finite element analysisFEM finite element methodFEPA Federation of European Producers
of AbrasivesFET field effect transistorsFFP fitness for purposeFIB focused ion beamFID flame ionization detectorFID free-induction decayFISH fluorescence in situ hybridizationFLAPW full potential linearized augmented
plane waveFNAA neutron activation analysisFPD flame photometric detectorFT Fourier transformFTS Fourier transform spectrometerFVM finite volume methodFWM four-wave mixing
G
GC gas chromatographyGC/MS gas chromatography with subsequent
mass spectrometryGC-IR gas chromatography–infraredGDP gross domestic productGGA generalized gradient approximationGLS Galerkin/least squares schemeGMI giant magnetoimpedance effectGMR giant magnetoresistanceGMRES generalized minimal residualGSED gaseous secondary electron detectorGVD group velocity dispersion
H
HCF high cycle fatiguehcp hexagonal-close-packedHGW hollow grass waveguideHISCC cathodic stress corrosion crackingHL hydrodynamically lubricatedHPLC high-performance liquid chromatographyHRR heat release rateHSA hemispherical analyzerHTS high-temperature superconductors
I
IAQ indoor air qualityIBRG International Biodeterioration
Research GroupIC ion chromatographyICP inductively coupled plasmaICP-OES ICP optical emission spectrometryICPS inductively coupled plasma
spectrometryICR ion cyclotron resonanceILAC International Laboratory Accreditation
CooperationILC inter-laboratory comparisonsIR infrared regionISO International Organization for
Standardization
J
JIS Japanese Standardization Organization
K
KC key comparisonsKKS Kim–Kim–Suzuki model
L
LC liquid chromatographyLCF low cycle fatigueLD laser diodeLDV laser Doppler velocimeterLED light-emitting diodeLIF laser-induced fluorescenceLOC limit of decisionLOD limit of detectionLOD limit of determinationLOQ limit of quantificationLSDA local spin density approximationLST linear system theoryLTS low-temperature superconductorsLVDT linear variable differential transformer
M
MAD median absolute deviationMD multichannel detectorMDM minimum detectable massMEMS micro-electromechanical systemsMIC microbially induced corrosionMIS metal–insulator–semiconductor structuresMITI Ministry of International Trade
and Industry of JapanMLLSQ multiple linear least squaresMMF minimum mass fraction
List of Abbreviations XXV
MOE modulus of elasticityMOKE magnetooptic Kerr effectMOS metal–oxide–semiconductorMRA recognition arrangementMRAM magnetic solid-state memoryMRAM magnetic random access memoryMS mass spectrometerMXCD magnetic X-ray circular dichroism
N
NAA neutron activation analysisNAB national accreditation bodiesNDP neutron depth profilingNEP noise-equivalent powerNHE normal hydrogen electrodeNIR near infraredNIST National Institute of Standards
and TechnologyNMI National Metrology InstituteNMR nuclear magnetic resonance
O
OA operational amplifierODS octadecylsilaneOECD Organization for Economic Cooperation
and DevelopmentOES optical emission spectrometryOKE optical Kerr effectOPG optical parametric generationOPO optical parametric oscillatorOR optical rectificationOTDR optical time-domain reflectometry
P
PA polyamidesPAC perturbed angular correlationsPAH polycyclic aromatic hydrocarbonPC photoconductivePCR polymerase chain reactionPE-HD high-density polyethylenePEELS parallel electron energy loss spectroscopyPEM photoelectromagneticPFM pulse field magnetometerPID photoionization detectorPIXE particle-induced X-ray emissionPL photoluminescencePMT photomultiplier tubePOD probability of detectionPT phototubePTFE polytetrafluoroethylenePV photovoltaicPVC polyvinyl chloridePWM pulse-width modulation
Q
QA quality assuranceQC quality controlQMR quasiminimal residual method
R
RAPD random amplified polymorphic DNARD rolling directionRDE rotating disc electrodeRE reference electrodeRF radiofrequencyRFLP restriction fragment length
polymorphismRH relative humidityRM reference materialsRMS root mean squareRPLC reversed-phase liquid chromatographyRRDE rotating ring disc electroderRNA ribosomal RNARSF relative sensitivity factor
S
S/N signal-to-noise ratioSAQCS sampling and analytical quality
control schemeSBS sick-building syndromeSBS stimulated Brillouin scatteringSCE saturated Calomel electrodeSCLM scanning confocal laser microscopySDD silicon drift detectorSEC specific energy consumptionSEM scanning electron microscopeSENB4 four-point single-edge notch bendSER specific emission ratesSFG sum-frequency generationSFM scanning force microscopySHE standard hydrogen electrodeSHG second-harmonic generationSNOM scanning near-field optical
microscopySOR successive overrelaxationSPH smooth particle hydrodynamics
methodSPT sampling proficiency testSQUID superconducting quantum
interference deviceSRE stray radiant energySRET scanning reference electrode
techniqueSRS stimulated Raman scatteringSST single-sheet testerSTEM scanning transmission electron
microscope
XXVI List of Abbreviations
STL stereolithographic data formatSTM scanning tunneling microscopesSUPG streamline-upwind Petrov–Galerkin
methodSVET scanning vibrating electrode technique
T
TAC time-to-amplitude converterTCD thermal conductivity detectorTCSPC time-correlated single-photon countingTDS total dissolved solidsTEM transmission electron microscopeTGA-IR thermal gravimetric analysis–infraredTHG third-harmonic generationTMR tunnel magneto-resistanceTMS tetramethylsilaneTOF time-of-flightTPA two-photon absorptionTVOC total volatile organic compounds
U
UHV ultrahigh vacuumUNI Ente Nationale Italiano di UnificazioneUT ultrasonic techniqueUVSG UV Spectrometry Group
V
VAMAS Versailles project on advanced materialsand standards
VOC volatile organic carbonVSM vibrating-sample magnetometer
W
WDM wavelength division multiplexingWDS wavelength dispersive spectrometerWFI water for injection
X
XAS X-ray absorption spectroscopyXPS X-ray photoelectron spectroscopyXRD X-ray diffractionXRF X-ray-fluorescence
Y
YAG yttrium aluminium garnet
Z
ZRA zero-resistance ammeter
1
MaterialsMPart APart A Materials Measurement System
1 Measurement Principles and StructuresAndrew Wallard, Sèvres, France
2 Measurement Strategy and QualityMichael H. Ramsey, Brighton, UKNick Boley, Teddington, UKStephen L.R. Ellison, Middlesex, UKWerner Hässelbarth, Berlin, GermanyHanspeter Ischi, Berne, SwitzerlandWolfhard Wegscheider, Leoben, AustriaAdolf Zschunke, Leipzig, Germany
3 Materials and Their Characteristics: OverviewHorst Czichos, Berlin, Germany
3
Measurement1. Measurement Principles and Structures
Part A of this handbook introduces the materialsmeasurement system, proceeding from general tospecific aspects:
• The present chapter describes the basic ele-ments of metrology, the system that allowsmeasurements made in different laborato-ries to be confidently compared. As the aimof this chapter is to give an overview of thewhole field, the development of metrologyfrom its roots to the birth of the meter con-vention and metrology in the 21st century isgiven.• Chapter 2 deals with measurement strategyand quality and presents the elements re-quired to make reliable measurements. Thisincludes sampling, traceability, comparability,accuracy, measurement uncertainty, referenceprocedures, and human aspects in a laboratory.• Chapter 3 reviews the basic features of materialsas a basis for the classification of the variousmethods used to characterize materials byanalysis, measurement, testing, modeling, andsimulation.
1.1 What Is Metrology? ............................... 3
1.2 The Roots and Evolution of Metrology .... 3
1.3 BIPM: The Birth of the Meter Convention 6
1.4 BIPM: The First 75 Years......................... 7
1.5 Quantum Standards: A MetrologicalRevolution ........................................... 8
1.6 Regional Metrology Organizations .......... 9
1.7 Traceability of Measurements ................ 10
1.8 Mutual Recognition of NMI Standards:The CIPM MRA ....................................... 101.8.1 The Essential Points of the MRA ...... 111.8.2 The Key Comparison Database
(KCDB) ......................................... 121.8.3 Take Up of the CIPM MRA ............... 12
1.9 Metrology in the 21st Century................. 121.9.1 Industrial Challenges .................... 121.9.2 Chemistry, Pharmacy
and Medicine .............................. 141.9.3 Environment, Public Services
and Infrastructures....................... 14
1.10 The SI System and New Science .............. 14
References .................................................. 16
1.1 What Is Metrology?
Metrology is generally defined as the “science of meas-urement.” This, of course, includes its application toa huge range of measurements in science, industry, theenvironment, as well as in healthcare or food quality;metrology is all around each and every one of us. Mea-surement provides us with a reference for our daily lifein the measurement of time, weight, length and all thehundreds of measurements that influence us.
In this general introduction to the subject, we shallfirst look at some of the early measurements and the
need to put them on a sound basis, and then reviewthe development of the worldwide system of standards.We will then take a look at the institutions and in-frastructure which now exists to coordinate accuratemeasurement throughout the world and the acceptanceof such measurements by those who need to use them.Finally, some of the new and emerging trends and is-sues which characterize the subject and which bringtheir own scientific, economic or social challenges areaddressed.
1.2 The Roots and Evolution of Metrology
From the earliest times it has been important to comparethings through measurements. This had much to do with
fair exchange, barter, or trade between communities andsimple weights such as the stone or measures such as
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4 Part A The Materials Measurement System
the cubit were common. At this level, parts of the bodysuch as hands and arms were adequate for most needs.Initially, wooden length bars were easy to compare andweights could be weighed against each other. Variousforms of balance were commonplace in early history andin religion. Egyptian tomb paintings show the Egyptiangod Anubis weighing the soul of the dead against an os-trich feather – the sign of purity (Fig. 1.1). Noah’s Arkwas, so the book of Genesis reports, 300 cubits long, by50 cubits wide and 30 cubits high. No one really knowswhy it was important to record such details but the Bible,as just one example, is littered with metrological refer-ences and the symbolism of metrology was part of earlyculture and art.
A steady progression from basic artifacts to naturallyoccurring reference standards has been part of the entirehistory of metrology. Metrologists are familiar with theuse of the carob seed in the early Mediterranean civi-
Fig. 1.1 Anubis
Fig. 1.2 Winchester Yard
lizations as a natural reference for length and for weightand hence volume. The Greeks were early traders whopaid attention to metrology and they were known to keepcopies of the weights and measures of the countries withwhich they traded.
The Magna Carta of England set out a framework fora citizen’s rights and established “one measure through-out the land.” Kings and queens took interest in nationalweights and measures, Fig. 1.2 shows the Winchesteryard, the bronze rod that was the British standard from1497 to the end of the 16th century. The queen’s markwe see here is that of Elizabeth the First (1558–1603).In those days, the acre was widely used as a measure-ment and derived from the area that a team of oxen couldplough in a day. Ploughing an acre meant that you had towalk 66 furlongs, a linear dimension measured in rods.
The problem with many length measurements wasthat the standard was made of the commonly availablemetals brass or bronze, which have a fairly large co-efficient of expansion. Iron or steel measures were notdeveloped for a couple of centuries. Brass and bronzetherefore dominated the length reference business untilthe early 19th century by which time metallurgy had de-veloped well enough – though it was still something ofa black art – for new, lower-expansion metals to be usedand reference temperatures quoted. The UK imperialreferences were introduced in 1854 and reproduced inTrafalgar Square in the center of London (Fig. 1.3) andthe British Empire’s domination of international com-merce saw the British measurement system adopted inmany of its colonies.
In the mid 18th century, Britain and France com-pared their national measurement standards and realizedthat they differed by a few percent for the same unit.Although the British system was reasonably consistentthroughout the country, the French found that differ-ences of up to 50% were common in length measurementwithin France. The ensuing technical debate was the startof what we now accept as the metric system. France ledthe way, and even in the middle of the French revolutionthe Academy of Science was asked to “deduce an invari-able standard for all the measures and all the weights.”The important word was “invariable.” There were twooptions available for the standard of length: the seconds’pendulum and the length of the earth’s meridian. The ob-vious weakness of the pendulum approach was that itsperiod depended on the local acceleration due to grav-ity. The Academy therefore chose to measure a portionof the earth’s circumference and relate it to the officialFrench meter. Delambre and Méchain, who were en-trusted with a survey of the meridian between Dunkirk
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Measurement Principles and Structures 1.2 The Roots and Evolution of Metrology 5
and Barcelona, created the famous Mètre des Archives,a platinum end standard.
The international nature of measurement was driven,just like that of the Greek traders of nearly 2000 yearsbefore, by the need for interoperability in trade and ad-vances in engineering measurement. The displays ofbrilliant engineering at the Great Exhibitions in Lon-don and Paris in the 19th century largely rested on theability to measure well. The British Victorian engineerJoseph Whitworth coined the famous phrase “you canonly make as well as you can measure” and pioneeredaccurate screw threads. He immediately saw the poten-tial of end standard gauges rather than line standardswhere the reference length was defined by a scratch onthe surface of a bar. The difficulty, he realized, with linestandards was that optical microscopes were not thengood enough to compare measurements of line stan-dards well enough for the best precision engineering.Whitworth was determined to make the world’s bestmeasuring machine. He constructed the quite remark-able “millionth machine” based on the principle thattouch was better than sight for precision measurement.It appears that the machine had a “feel” of about 1/10of a thousandth of an inch. Another interesting metro-logical trend at the 1851 Great Exhibition was military:the word “calibrate” comes from the need to control thecalibre of guns.
At the turn of the 19th century, many of the in-dustrialized countries had set up National MetrologyInstitutes, generally based on the model establishedin Germany with the Physikalisch Technische Reich-sanstalt, which was founded in 1887. The economicbenefits of such a national institute were immediatelyrecognized and, as a result, scientific and industrial orga-nizations in a number of industrialized countries beganpressing their Governments to make similar investments.In the UK, the British Association for the Advancementof Science reported that, without a national laboratoryto act as a focus for metrology, the country’s indus-trial competitiveness would be weakened. The cause wastaken up more widely and the UK set up the NationalPhysical Laboratory (NPL) in 1900. The US created theNational Bureau of Standards in 1901 as a result of sim-ilar industrial pressure. The major national metrologyinstitutes (NMIs), however, had a dual role. In general,they were the main focus for national research programson applied physics and engineering. Their scientific rolein the development of units – what became the Inter-national System of Units, the SI – began to challengethe role of the universities in the measurement of thefundamental constants. This was especially true after
Fig. 1.3 Imperial length standards. Trafalgar Square, London
the development of quantum physics in the 1920s and1930s. Most early NMIs therefore began with two majorelements to their mission:
• a requirement to satisfy industrial needs for ac-curate measurements, through standardization andverification of instruments; and• determining the physical constants so as to improveand develop the SI system.
The new industries which emerged after the First WorldWar made huge demands on metrology and, togetherwith mass production and the beginnings of multina-tional production sites, raised new challenges whichbrought NMIs into direct contact with companies, socausing a close link to develop between them. At thattime, and even up to the mid 1960s, nearly all cal-ibrations and measurements that were necessary forindustrial use were made in the NMIs, and in the gaugerooms of the major companies, as most measurementswere in engineering metrology. The industries of the1920s, however, developed a need for electrical and op-tical measurements so NMIs expanded their coverageand their technical abilities.
The story since then is one of steady technical ex-pansion until after the Second World War. In the 1950s,though, there was a renewed interest in a broader ap-plied focus for many NMIs so as to develop civilianapplications for much of the declassified military tech-nology. The squeeze on public budgets in the 1970sand 1980s saw a return to core metrology and manyother institutions, public and private, took on the re-sponsibility for developing many of the technologies,which had been initially fostered at NMIs. The NMIsadjusted to their new roles. Many restructured andfound new, often improved, ways of serving indus-trial needs. This recreation of the NMI role was alsoshared by most Governments, which increasingly saw
PartA
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6 Part A The Materials Measurement System
them as tools of industrial policy with a mission tostimulate industrial competitiveness and, at the end of
the 20th century, to reduce technical barriers to worldtrade.
1.3 BIPM: The Birth of the Meter Convention
During the 1851 Great Exhibition and the 1860 meet-ing of the British Association for the Advancement ofScience (BAAS) a number of scientists and engineersmet to develop the case for a single system of unitsbased on the metric system. This built on the early ini-tiative of Gauss to use the 1799 meter and kilogram inthe Archives de la République, Paris and the second, asdefined in astronomy, to create a coherent set of unitsfor the physical sciences. In 1874, the three-dimensionalCGS system, based on the centimeter, gram and second,was launched by the BAAS. However, the size of theelectrical units in the CGS system were not particularlyconvenient and, in the 1880s, the BAAS and the Inter-national Electrotechnical Commission (IEC) approveda set of practical electrical units based on the ohm, theampere, and the volt. Parallel to this attention to the units,a number of governments set up what was then called theCommittee for Weights and Money, which in turn led tothe 1870 meeting of the Commission Internationale duMètre. Twenty-six countries accepted the invitation ofthe French Government to attend; however, only 16 wereable to come as the Franco–Prussian war intervened, sothe full committee did not meet until 1872. The resultwas the Convention du Mètre and the creation of the Bu-reau International des Poids et Mesures, the BIPM (inEnglish the International Bureau of Weights and Mea-sures), in the old Pavillon de Breteuil at Sèvres (Fig. 1.4),as a permanent scientific agency supported by the signa-tories to the convention. As this required the support of
Fig. 1.4 Bureau International des Poids et Mesures, Sérres
governments at the highest level the Meter Conventionwas not finally signed until 20th May 1875.
The BIPM’s role was to “establish new metric stan-dards, conserve the international prototypes” (then themeter and the kilogram) and “to carry out the compar-isons necessary to assure the uniformity of measuresthroughout the world.” As an intergovernmental, diplo-matic treaty organization, the BIPM was placed underthe authority of the General Conference on Weights andMeasures (CGPM). A committee of 18 scientific experts,the International Committee for Weights and Measures(CIPM), now supervises the running of the BIPM. Theaim of the CGPM and the CIPM was, and still is, to as-sure the “international unification and development ofthe metric system.” The CGPM now meets every fouryears to review progress, receive reports from the CIPMon the running of the BIPM and to establish the op-erating budget of the BIPM, whereas the CIPM meetsannually to supervise the BIPM’s work.
When it was set up, the staff of the BIPM consistedof a director, two assistants and the necessary number ofemployees. In essence, then, a handful of people beganto prepare and disseminate copies of the internationalprototypes of the meter and the kilogram to memberstates. About 30 copies of the meter and 40 copies of theprototype kilogram were distributed to member states byballot. Once this was done, some thought that the job ofthe BIPM would simply be that of periodically checking(in the jargon, verifying) the national copies of thesestandards. This was a short-lived vision as the earlyinvestigations immediately showed the importance ofreliably measuring a range of quantities that influencedthe performance of the international prototypes and theircopies. As a result, a number of studies and projectswere launched which dealt with the measurement oftemperature, density, pressure and a number of relatedquantities. The BIPM immediately became a researchbody, although this was not recognized formally until1921.
Returning to the development of the SI; one of theearly decisions of the CIPM was to modify the CGS sys-tem to base measurements on the meter, kilogram andsecond – the MKS system. In 1901, Giorgi showed that itwas possible to combine the MKS system with the prac-
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1.3
Measurement Principles and Structures 1.4 BIPM: The First 75 Years 7
tical electrical units to form a coherent four-dimensionalsystem by adding an electrical unit and rewriting someof the equations of electromagnetism in the so-called ra-tionalized form. In 1946, the CIPM approved a systembased on the meter, kilogram, second and ampere – theMKSA system. Recognizing the ampere as a base unitof the metric system in 1948, and adding, in 1954, unitsfor thermodynamic temperature (the kelvin) and lumi-nous intensity (the candela), the 11th CGPM in 1960coined the name Système internationale d’Unités, the
SI. At the 14th CGPM in 1971, the present day SI sys-tem was completed by adding the mole as the base unitfor the amount of substance, bringing the total numberof base units to seven. Using these base units, a hierar-chy of derived units and quantities of the SI have beendeveloped for most, if not all, measurements needed intoday’s society. A substantial treatment of the SI is tobe found in the SI brochure published by the BIPM inits seventh edition in 1998, with the publication of aneighth edition expected in 2005 [1.1].
1.4 BIPM: The First 75 Years
After its intervention in the initial development of theSI, the BIPM continued to develop fundamental metro-logical techniques in mass and length measurementbut soon had to react to the metrological implicationsof major developments in atomic physics and inter-ferometry. In the early 1920s, Albert Michelson cameto work at the BIPM and built an eponymous in-terferometer to measure the meter in terms of lightfrom the cadmium red line – an instrument which, al-though modified, did sterling service until the 1980s. Intemperature measurement, the old hydrogen thermome-ter scale was replaced with a thermodynamic-basedscale and a number of fixed points. After great de-bate, electrical standards were added to the work ofthe BIPM in the 1920s with the first internationalcomparisons of resistance and voltage. In 1929, an elec-trical laboratory was added and photometry arrived in1939.
In these early days, it was clear that the BIPM neededto find a way of consulting and collaborating with theexperts in the world’s NMIs. The solution adopted isone which still exists and flourishes today. The best wayof working was in face-to-face meetings, so the con-cept of a consultative committee to the CIPM was born.Members of the committee were drawn from experts ac-tive in the world’s NMIs and met to deal with mattersconcerning the definitions of units and the techniquesof comparison and calibration. The consultative com-mittees are usually chaired by a member of the CIPM.Much information was shared although, for obvious lo-gistical reasons, the meetings were not too frequent.Over the years, the need for new consultative committeesgrew in reaction to the expansion of metrology and nowten consultative committees exist, with over 25 workinggroups.
The CIPM is rightly cautious about establishinga new committee but proposals for new ones are con-sidered from time to time, usually after an initial surveythrough a working group. In the last ten years, jointcommittees have been created to tackle issues such as theinternational approach to the estimation of measurementuncertainties or to the establishment of a common vo-cabulary for metrology. Most of these joint committeesbring the BIPM together with international or intergov-ernmental bodies such as the International Organizationfor Standardization (ISO), the International LaboratoryAccreditation Cooperation (ILAC), and the IEC. As thework of the Meter Convention moves into areas otherthan its traditional activities in physics and engineer-ing, joint committees are an excellent way of bringingthe BIPM together with other bodies that bring special-ist expertise – an example being the joint committee forlaboratory medicine, established recently with the Inter-national Federation of Clinical Chemists and the ILAC.
The introduction of ionizing radiation standards tothe work of the BIPM came when Marie Curie depositedher first radium standard at the BIPM in 1913. As a re-sult of pressure, largely from the USSR delegation tothe CGPM, the CIPM took the decision to deal withmetrology in ionizing radiation.
In the mid 1960s, and at the time of the expansioninto ionizing radiation, programs on laser length mea-surement were also started. These contributed greatly tothe redefinition of the meter in 1983. The BIPM alsoacted as the world reference center for laser wavelengthor frequency comparisons in much the same was as itdid for physical artifact-based standards. In the mean-time, however, the meter bar had already been replaced,in 1960, by an interferometric-based definition usingoptical radiation from a krypton lamp.
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1.4
8 Part A The Materials Measurement System
Table 1.1 List of consultative committees with dates of formation
Names of consultative committees and the date of their formation
(Names of consultative committees have changed as they have gained new responsibilities: the current name iscited)
Consultative Committee for Electricity and Magnetism, CCEM. (1997, but created in 1927)
Consultative Committee for Photometry and Radiometry, CCPR. (1971 but created in 1933)
Consultative Committee for Thermometry, CCT (1937)
Consultative Committee for Length, CCL (1997 but created in 1952)
Consultative Committee for Time and Frequency, CCTF. (1997, but created 1956)
Consultative Committee for Ionizing Radiation, CCRI. (1997, but created in 1958)
Consultative Committee for Units, CCU. (1964, but replacing a similar commission created in 1954)
Consultative Committee for Mass and Related Quantities, CCM. (1980)
Consultative Committee for Amount of Substance and Metrology in Chemistry, CCQM. (1993)
Consultative Committee for Acoustics, Ultrasound and Vibration, CCAUV. (1999)
1.5 Quantum Standards: A Metrological Revolution
Technology did not stand still and, in reaction tothe developments and metrological applications of su-perconductivity, important projects on the Josephson,quantum Hall and capacitance standards were launchedin the late 1980s and 1990s. The BIPM played a key rolein establishing worldwide confidence in the performanceof these new devices through an intense program of com-parisons which revealed many of the systematic sourcesof error and found solutions to them. The emergence ofthese and other quantum-based standards, however, wasan important and highly significant development. In ret-rospect, these were one of the drivers for change in theway in which world metrology organizes itself and hadimplications nationally as well as internationally.
The major technical change was, in essence, a be-lief that standards based on quantum phenomena werethe same the world over. Their introduction sometimesmade it unnecessary for a single, or a small number of,reference standards to be held at the BIPM or in a few ofthe well-established and experienced NMIs. Quantum-based standards were, in reality, available to all and, withcare, could be operated outside the NMIs at very highlevels of accuracy.
There were two consequences. Firstly, that the newerNMIs that wanted to invest in quantum-based standardsneeded to work with experienced metrologists in exist-ing NMIs in order to develop their skills as rapidly as
possible. Many of the older NMIs, therefore, becameadept at training and providing the necessary experi-ence for newer metrologists. The second consequencewas an increased pressure for comparisons of standards,as the ever-conservative metrology community soughtto develop confidence in new NMIs as well as in thequantum-based standards. These included frequency-stabilized lasers, superconducting voltage and resistancestandards, cryogenic radiometers (for measurements re-lated to the candela), atomic clocks (for the second) anda range of secondary standards.
Apart from its responsibility to maintain the interna-tional prototype kilogram (Fig. 1.5), which remains thelast artifact-based unit of the SI, the BIPM was thereforeno longer always the sole repository of an internationalprimary reference standard. However there were, andstill are, a number of unique reference facilities at theBIPM for secondary standards and quantities of the SI.Staff numbers had also leveled off at about 70.
If it was going to maintain its original mission ofa scientifically based organization with the responsibilityfor coordinating world metrology, the BIPM recognizedit needed to discharge particular aspects of its treatyobligation in a different way. It also saw the increasedvalue of developing the links needed to establish col-laboration at the international and intergovernmentallevel. In addition, the staff had the responsibility to pro-
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1.5