BS ISO 13067-2011 Microbeam analysis Electron backscatter diffraction Measurement of average grain size《微光束分析 背散射电子衍射 平均颗粒粒度测量》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 13067:2011Microbeam analysis Electron backscatter diffraction Measurement of average grain sizeBS ISO 13067:2011 BRITISH STANDARDNational forewordThis British Standard is

2、the UK implementation of ISO 13067:2011.The UK participation in its preparation was entrusted to TechnicalCommittee CII/9, Microbeam analysis.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessar

3、yprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 65773 3ICS 71.040.50Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committe

4、e on 30 November 2011.Amendments issued since publicationDate Text affectedBS ISO 13067:2011Microbeam analysis Electron backscatter diffraction Measurement of average grain sizeAnalyse par microfaisceaux Diffraction dlectrons rtrodiffuss Mesurage de la taille moyenne des grainsISO13067BS ISO 13067:2

5、011ISO 13067:2011(E)COPYRIGHT PROTECTED DOCUMENTBS ISO 13067:2011ISO 13067:2011(E)Contents Foreword ivIntroduction v1 Scope 12 Normative references .13 Terms and definitions .13.1 Terminology associated with EBSD measurement of grain size 13.2 Terminology associated with grains and grain boundaries

6、determined via EBSD .33.3 Terminology associated within grain size measurement .43.4 Terminology associated with data correction and uncertainty of EBSD maps 54 Acquiring a map by EBSD for grain size measurement .54.1 Hardware requirements .54.2 Software requirements .65 Acquiring the map for grain

7、sizing by EBSD .65.1 Specimen preparation 65.2 Defining specimen axes 65.3 Stage positioning and calibration .65.4 Linear calibration .65.5 Preliminary examination 75.6 Choice of step size 75.7 Determination of the level of angular accuracy needed .75.8 Choice of areas to be mapped and map size .95.

8、9 Considerations when examining plastically deformed materials 96 Analytical procedure 106.1 Definition of boundaries 106.2 Post-acquisition treatment of raw data .116.3 Data-cleaning steps 116.4 Measurement of grain size 146.5 Representation of data .147 Measurement uncertainty .158 Reporting of an

9、alysis results .15Annex A Grain size measurement .16Bibliography .18BS ISO 13067:2011ForewordMicrobeam analysisISO 13067:2011(E)BS ISO 13067:2011IntroductionISO 13067:2011(E)BS ISO 13067:2011BS ISO 13067:2011INTERNATIONAL STANDARD ISO 13067:2011(E)Microbeam analysis Electron backscatter diffraction

10、Measurement of average grain sizeIMPORTANT The electronic file of this document contains colours which are considered to be useful for the correct understanding of the document. Users should therefore consider printing this document using a colour printer.1 Scope2 Normative referencesMicrobeam analy

11、sis Scanning electron microscopy Guidelines for calibrating image magnificationGeneral requirements for the competence of testing and calibration laboratoriesGuidance for the use of repeatability, reproducibility and trueness estimates in measurement uncertainty estimationMicrobeam analysis Electron

12、 probe microanalysis (EPMA) VocabularyMicrobeam analysis Guidelines for orientation measurement using electron backscatter diffraction3 Terms and definitions3.1 Terminology associated with EBSD measurement of grain size3.1.1step size1BS ISO 13067:20113.1.2pixelpicture element3.1.3orientation3.1.4ind

13、exed3.1.5indexing reliability3.1.6orientation mapcrystal orientation map3.1.7pattern quality3.1.8pattern quality map3.1.9pseudosymmetryISO 13067:2011(E)2 BS ISO 13067:2011c/a3.1.10misorientation3.1.11disorientation3.1.12forescatter imaging3.1.13electron-channelling contrast imagingECCI3.1.14barrel d

14、istortion3.1.15pincushion distortion3.2 Terminology associated with grains and grain boundaries determined via EBSD3.2.1grain boundary3.2.2grain3.2.3sub-grain boundaryISO 13067:2011(E)3BS ISO 13067:20113.2.4sub-grain3.2.5special boundary3.2.6twin boundary3.2.7recrystallized grains3.2.8phase3.3 Termi

15、nology associated within grain size measurement3.3.1line intercept3.3.2equivalent circle diameterDD = A AGG = D DISO 13067:2011(E)4 BS ISO 13067:20113.3.3Feret diameter3.3.4grain shape3.3.5grain shape orientation3.4 Terminology associated with data correction and uncertainty of EBSD maps3.4.1misinde

16、xing3.4.2non-indexing3.4.3data cleaning4 Acquiring a map by EBSD for grain size measurement4.1 Hardware requirementsISO 13067:2011(E)5BS ISO 13067:20114.2 Software requirements4.2.1 4.2.2 4.2.3 4.2.4 5 Acquiring the map for grain sizing by EBSD5.1 Specimen preparation5.2 Defining specimen axes5.3 St

17、age positioning and calibration5.4 Linear calibrationISO 13067:2011(E)6 BS ISO 13067:20115.5 Preliminary examination5.6 Choice of step size5.6.15.6.25.6.35.7 Determination of the level of angular accuracy neededISO 13067:2011(E)7BS ISO 13067:2011a) b)c) d)e) f)Figure 1 An area of an Ni superalloy ma

18、pped by EBSD under different conditionsISO 13067:2011(E)8 BS ISO 13067:2011 5.8 Choice of areas to be mapped and map size5.9 Considerations when examining plastically deformed materialsISO 13067:2011(E)9BS ISO 13067:20116 Analytical procedure6.1 Definition of boundaries6.1.1 Grain boundary angles6.1

19、.2 Handling incomplete boundaries6.1.3 Dealing with special boundaries.ISO 13067:2011(E)10 BS ISO 13067:20116.2 Post-acquisition treatment of raw data6.3 Data-cleaning steps6.3.16.3.2 xx6.3.3 6.3.46.3.5ISO 13067:2011(E)11BS ISO 13067:20116.3.66.3.7KeyFigure 2 Cumulative grain size distributions resu

20、lting from different data-cleaning methodsISO 13067:2011(E)12 BS ISO 13067:2011Table 1 Mean values for grain size, i.e. circle equivalent diameter, from the graphs shown in Figure 2 to illustrate the differences in measured average grain size depending on the data-cleaning method chosenData-cleaning

21、 method Size Number Size Number Size NumberKeyFigure 3 Cumulative grain size distributions resulting from different map step sizes and single-pixel removal during data cleaningISO 13067:2011(E)13BS ISO 13067:2011KeyFigure 4 Cumulative grain size distributions resulting from different map step sizes

22、and removal of grains with two or fewer neighbours during data cleaning6.4 Measurement of grain size6.5 Representation of dataISO 13067:2011(E)14 BS ISO 13067:20117 Measurement uncertainty8 Reporting of analysis results8.1 8.2 8.3 8.4 ISO 13067:2011(E)15BS ISO 13067:2011Annex A Grain size measuremen

23、tDQuantitative Microscopy= AA D=piD A A= = = piISO 13067:2011(E)16 BS ISO 13067:2011ISO 13067:2011(E)17BS ISO 13067:2011Bibliographyandle Microtexture Determination and Its ApplicationsumphreysJ. Mater. Sci. 36iles Stochastic Geometryantujoul Microscopica Acta 5rightPractische Metallographie 47umphr

24、eys ate urleyJ. Microscopy 201ngler andle Introduction to Texture Analysisright adams Metall. Trans. A 23right arsenJ. Microscopy 205ay uestedJ. Microscopy195rimby rior heeler ,J. Structural Geol. 20alcke ennock rury e esserJ. Microscopy 224olze Ultramicroscopy107Standard Test Methods for Determinin

25、g Average Grain SizeStandard Test Methods for Estimating the Largest Grain Observed in a Metallographic Section (ALA Grain Size)Standard Test Methods for Characterizing Duplex Grain SizesStandard Test Methods for Determining Average Grain Size Using Semiautomatic and Automatic Image AnalysisAdvanced

26、 technical ceramics Monolithic ceramics General and textural properties Part 3: Determination of grain size and size distribution (characterized by the Linear Intercept Method)e off hines Quantitative MicroscopyxnerPowder Metall. 13 (26)ander oort rielMaterials Characterisation 29ISO 13067:2011(E)18 BS ISO 13067:2011BS ISO 13067:2011ISO 13067:2011(E)ICS 71.040.50This page deliberately left blank