EN ISO 13383-2-2016 en Fine ceramics (advanced ceramics advanced technical ceramics) - Microstructural characterization - Part 2 Determination of phase volume fraction by evaluatio.pdf

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1、BS EN ISO 13383-2:2016Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterizationPart 2: Determination of phase volume fraction by evaluation of micrographs (ISO 13383-2:2012)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN IS

2、O 13383-2:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 13383-2:2016. It is identical to ISO 13383-2:2012. It supersedes BS EN 623-5:2009 and BS ISO 13383-2:2012 which are withdrawn.The UK participation in its preparation was entrusted to Technical Co

3、mmittee RPI/13, Advanced technical ceramics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standa

4、rds Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 91171 2ICS 81.060.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2012

5、.Amendments/corrigenda issued since publicationDate Text affected31 May 2016 This corrigendum renumbers BS ISO 13383-2:2012 as BS EN ISO 13383-2:2016EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13383-2 April 2016 ICS 81.060.30 Supersedes EN 623-5:2009English Version Fine ceramics (advanc

6、ed ceramics, advanced technical ceramics) - Microstructural characterization - Part 2: Determination of phase volume fraction by evaluation of micrographs (ISO 13383-2:2012) Cramiques techniques - Caractrisation microstructurale - Partie 2: Dtermination de la fraction volumique des phases par valuat

7、ion de micrographies (ISO 13383-2:2012) Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 2: Bestimmung des Volumenanteils von Phasen durch Auswertung von Mikrogefgeaufnahmen (ISO 13383-2:2012) This European Standard was approved by CEN on 19 March 2016. CEN members are bound to comp

8、ly with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC

9、 Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the sa

10、me status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg

11、, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 201

12、6 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13383-2:2016 EBS ISO 13383-2:2012ISO 13383-2:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 24 Appa

13、ratus . 24.1 Sectioning equipment . 24.2 Mounting equipment . 24.3 Grinding and polishing equipment 24.4 Microscope . 24.5 Transparent grid 25 Test piece preparation 35.1 Sampling . 35.2 Cutting 35.3 Mounting 35.4 Grinding and polishing . 35.5 Etching . 36 Photomicrography 46.1 General aspects . 46.

14、2 Inspection 46.3 Number of micrographs 46.4 Optical microscopy 46.5 Scanning electron microscopy . 57 Measurement of micrographs . 58 Calculation of results . 69 Interferences and uncertainties . 610 Test report . 7Annex A (informative) Use of automatic image analysis (AIA) 9Annex B (informative) R

15、ound-robin verification of this procedure .10Annex C (informative) Results sheet ISO 13383-2 .11Bibliography .12BS EN ISO 13383-2:2016EN ISO 13383-2:2016 (E)EN ISO 13383-2:2016 (E) 3 European foreword The text of ISO 13383-2:2012 has been prepared by Technical Committee ISO/TC 206 “Fine ceramics” of

16、 the International Organization for Standardization (ISO) and has been taken over as EN ISO 13383-2:2016 by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publica

17、tion of an identical text or by endorsement, at the latest by October 2016, and conflicting national standards shall be withdrawn at the latest by October 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC sh

18、all not be held responsible for identifying any or all such patent rights. This document supersedes EN 623-5:2009. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulga

19、ria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Tur

20、key and the United Kingdom. Endorsement notice The text of ISO 13383-2:2012 has been approved by CEN as EN ISO 13383-2:2016 without any modification. BS ISO 13383-2:2012ISO 13383-2:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definiti

21、ons . 24 Apparatus . 24.1 Sectioning equipment . 24.2 Mounting equipment . 24.3 Grinding and polishing equipment 24.4 Microscope . 24.5 Transparent grid 25 Test piece preparation 35.1 Sampling . 35.2 Cutting 35.3 Mounting 35.4 Grinding and polishing . 35.5 Etching . 36 Photomicrography 46.1 General

22、aspects . 46.2 Inspection 46.3 Number of micrographs 46.4 Optical microscopy 46.5 Scanning electron microscopy . 57 Measurement of micrographs . 58 Calculation of results . 69 Interferences and uncertainties . 610 Test report . 7Annex A (informative) Use of automatic image analysis (AIA) 9Annex B (i

23、nformative) Round-robin verification of this procedure .10Annex C (informative) Results sheet ISO 13383-2 .11Bibliography .12BS EN ISO 13383-2:2016ISO 13383-2:2012(E)BS ISO 13383-2:2012ISO 13383-2:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of na

24、tional standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. Intern

25、ational organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the r

26、ules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at

27、 least 75 % of the member bodies casting a vote.ISO 13383-2 was prepared by Technical Committee ISO/TC 206, Fine ceramics.ISO 13383 consists of the following parts, under the general title Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterization: Part 1: Determ

28、ination of grain size and size distribution Part 2: Determination of phase volume fraction by evaluation of micrographsiv ISO 2012 All rights reservedBS ISO 13383-2:2012INTERNATIONAL STANDARD ISO 13383-2:2012(E)Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characteri

29、zation Part 2: Determination of phase volume fraction by evaluation of micrographs1 ScopeThis part of ISO 13383 specifies a manual method of making measurements for the determination of the volume fraction of major phases in fine ceramics (advanced ceramics, advanced technical ceramics) using microg

30、raphs of polished and etched sections, overlaying a square grid of lines, and counting the number of intersections lying over each phase.NOTE 1 This method assumes that the true phase volume fractions are equivalent to area fractions on a randomly cut cross-section according to stereological princip

31、les.NOTE 2 Guidelines for polishing and etching of advanced technical ceramics can be found in Annexes A and B of ISO 13383-1:2012.The method applies to ceramics with one or more distinct secondary phases, such as found in Al2O3/ZrO2, Si/SiC, or Al2O3/SiCw.If the test material contains discrete pore

32、s, these are to be treated as a secondary phase for the purpose of this method, provided that there is no evidence of grain pluck-out during polishing being confused with genuine pores.NOTE 3 If the material contains more than about 20 % porosity, there is a strong risk that the microstructure will

33、be damaged during the polishing process, and measurement of the volume fraction of pores may become misleading. Secondary phase volume fractions or porosity present at levels of less than 0,05 are subject to considerable error and potential scatter in results. A larger number of micrographs than the

34、 minimum of three is normally needed to improve the consistency and accuracy of the results.NOTE 4 Many ceramics contain small amounts of secondary glassy phases. In order to make a reasonable estimate of glassy phase content, the glass material between crystalline grains should be readily observabl

35、e, and thus should be at least 0,5 m in width. The method in this part of ISO 13383 is not considered appropriate for narrow glassy films around grains.NOTE 5 Microstructures are seldom homogeneous, and the phase contents can vary from micrograph to micrograph. It is essential to survey a sufficient

36、ly wide area of the prepared section to ensure that those areas selected for evaluation are representative, and do not contain eye-catching irregularities. This method assumes that the selected regions of a prepared cross-section are statistically representative of the whole sampled section.Some use

37、rs of this part of ISO 13383 may wish to apply automatic or semiautomatic image analysis to micrographs or directly captured microstructural images. This is currently outside the scope of this part, but some guidelines are given in Annex A.2 Normative referencesThe following referenced documents are

38、 indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO/IEC 17025, General requirements for the competence of testing and calibration labora

39、tories ISO 2012 All rights reserved 1BS EN ISO 13383-2:2016ISO 13383-2:2012(E)BS ISO 13383-2:2012ISO 13383-2:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standar

40、ds is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take

41、 part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to

42、 prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.ISO 13383-2 was prepared by Technical Co

43、mmittee ISO/TC 206, Fine ceramics.ISO 13383 consists of the following parts, under the general title Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterization: Part 1: Determination of grain size and size distribution Part 2: Determination of phase volume fracti

44、on by evaluation of micrographsiv ISO 2012 All rights reservedBS ISO 13383-2:2012INTERNATIONAL STANDARD ISO 13383-2:2012(E)Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterization Part 2: Determination of phase volume fraction by evaluation of micrographs1 Scop

45、eThis part of ISO 13383 specifies a manual method of making measurements for the determination of the volume fraction of major phases in fine ceramics (advanced ceramics, advanced technical ceramics) using micrographs of polished and etched sections, overlaying a square grid of lines, and counting t

46、he number of intersections lying over each phase.NOTE 1 This method assumes that the true phase volume fractions are equivalent to area fractions on a randomly cut cross-section according to stereological principles.NOTE 2 Guidelines for polishing and etching of advanced technical ceramics can be fo

47、und in Annexes A and B of ISO 13383-1:2012.The method applies to ceramics with one or more distinct secondary phases, such as found in Al2O3/ZrO2, Si/SiC, or Al2O3/SiCw.If the test material contains discrete pores, these are to be treated as a secondary phase for the purpose of this method, provided

48、 that there is no evidence of grain pluck-out during polishing being confused with genuine pores.NOTE 3 If the material contains more than about 20 % porosity, there is a strong risk that the microstructure will be damaged during the polishing process, and measurement of the volume fraction of pores

49、 may become misleading. Secondary phase volume fractions or porosity present at levels of less than 0,05 are subject to considerable error and potential scatter in results. A larger number of micrographs than the minimum of three is normally needed to improve the consistency and accuracy of the results.NOTE 4 Many ceramics contain small amounts of secondary glassy phases. In order to make a reasonable estimate of glassy phase content, the glass material between crystalline grains should be readily observable, and thus should be at least 0