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

1、August 2016 English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 81.060.30!%Y.;“2541124www.din.deD

2、IN EN ISO 13383-2Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterization Part 2: Determination of phase volume fraction by evaluation of micrographs (ISO 13383-2:2012);English version EN ISO 13383-2:2016,English translation of DIN EN ISO 13383-2:2016-08Hochlei

3、stungskeramik Mikrostrukturelle Charakterisierung Teil 2: Bestimmung des Volumenanteils von Phasen durch Auswertung von Mikrogefgeaufnahmen (ISO 13383-2:2012);Englische Fassung EN ISO 13383-2:2016,Englische bersetzung von DIN EN ISO 13383-2:2016-08Cramiques techniques Caractrisation microstructurale

4、 Partie 2: Dtermination de la fraction volumique des phases par valuation de micrographes (ISO 13383-2:2012);Version anglaise EN ISO 13383-2:2016,Traduction anglaise de DIN EN ISO 13383-2:2016-08SupersedesDIN EN 623-5:2009-10www.beuth.deDocument comprises 20 pagesDTranslation by DIN-Sprachendienst.I

5、n case of doubt, the German-language original shall be considered authoritative.08.16 DIN EN ISO 13383-2:2016-08 2 A comma is used as the decimal marker. National foreword The text of ISO 13383-2:2012 has been prepared by Technical Committee ISO/TC 206 “Fine ceramics” and has been taken over as EN I

6、SO 13383-2:2016 by Technical Committee CEN/TC 184 “Advanced technical ceramics” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-02-91 AA Terminologie von

7、Hochleistungskeramik und Prfung von monolithischen keramischen Werkstoffen und Pulvern. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 6106:2005 DIN ISO 6106:2006-03 ISO 8486-1:1996 DIN ISO 8486-1:1997-09 ISO 8486-2:1996 DIN ISO 8486-2

8、:1997-09 ISO/IEC 17025 DIN EN ISO/IEC 17025 Amendments This standard differs from DIN EN 623-5:2009-10 as follows: a) a figure has been added to Clause 7 “Measurement of micrographs” for purposes of clarification; b) the Annexes “Grinding and polishing procedures”, “Etching procedures”, and “Setting

9、 Khler illumination in an optical microscope”, which are included in DIN EN 623-3 and DIN EN 623-5 are also given in DIN EN ISO 13383-1, and thus are not repeated in DIN EN ISO 13383-2; c) the Bibliography has been updated. Previous editions DIN V ENV 623-5: 2002-10 DIN EN 623-5: 2009-10 DIN EN ISO

10、13383-2:2016-08 3 National Annex NA (informative) Bibliography DIN EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories DIN ISO 6106:1996-03, Abrasive products Checking the grain size of superabrasives DIN ISO 8486-1:1997-09, Bonded abrasives Determinatio

11、n and designation of grain size distribution Part 1: Macrogrits F4 to F220 DIN ISO 8486-2:1997-09, Bonded abrasives Determination and designation of grain size distribution Part 2: Microgrits F230 to F2000 DIN EN ISO 13383-2:2016-08 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENN

12、E EUROPISCHE NORM EN ISO 13383-2 April 2016 ICS 81.060.30 Supersedes EN 623-5:2009English Version Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural characterization - Part 2: Determination of phase volume fraction by evaluation of micrographs (ISO 13383-2:2012) Cramiqu

13、es techniques - Caractrisation microstructurale - Partie 2: Dtermination de la fraction volumique des phases par valuation de micrographes (ISO 13383-2:2012) Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 2: Bestimmung des Volumenanteils von Phasen durch Auswertung von Mikrogefgea

14、ufnahmen (ISO 13383-2:2012) This European Standard was approved by CEN on 19 March 2016. CEN members are bound to comply 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 lis

15、ts and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC 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

16、 the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yu

17、goslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPE

18、N DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 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 EContents PageForeword 41 Scope .52 Normative

19、references 53 Terms and definitions .64 Apparatus .64.1 Sectioning equipment .64.2 Mounting equipment .64.3 Grinding and polishing equipment 64.4 Microscope .64.5 Transparent grid 65 Test piece preparation 75.1 Sampling .75.2 Cutting 75.3 Mounting 75.4 Grinding and polishing .75.5 Etching .76 Photom

20、icrography 86.1 General aspects .86.2 Inspection 86.3 Number of micrographs 86.4 Optical microscopy 86.5 Scanning electron microscopy .97 Measurement of micrographs .98 Calculation of results .109 Interferences and uncertainties .1010 Test report .11Annex A (informative) Use of automatic image analy

21、sis (AIA)13Annex B (informative) Round-robin verification of this procedure .14Annex C (informative) Results sheet ISO 13383-2 .15Bibliography .162EN ISO 13383 2:2016 (E) -DIN EN ISO 13383-2:2016-08 European foreword 3European foreword The text of ISO 13383-2:2012 has been prepared by Technical Comm

22、ittee ISO/TC 206 “Fine ceramics” of 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 n

23、ational standard, either by publication 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 p

24、atent rights. CEN and/or CENELEC shall 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 Europea

25、n Standard: 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, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloven

26、ia, Spain, Sweden, Switzerland, Turkey 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. 3EN ISO 13383 2:2016 (E) -DIN EN ISO 13383-2:2016-08 ForewordISO (the International Organization for Standardizatio

27、n) is a worldwide federation of national 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 rep

28、resented on that committee. International 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 ar

29、e drafted in accordance with the rules 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 Internationa

30、l Standard requires approval by at 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) Microstructura

31、l characterization: Part 1: Determination of grain size and size distribution Part 2: Determination of phase volume fraction by evaluation of micrographs4EN ISO 13383 2:2016 (E) -DIN EN ISO 13383-2:2016-08 1 ScopeThis part of ISO 13383 specifies a manual method of making measurements for the determi

32、nation 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 the number of intersections lying over each phase.NOTE 1 This method assumes that the tru

33、e 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 found in Annexes A and B of ISO 13383-1:2012.The method applies to ceramics with one or mo

34、re 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 that there is no evidence of grain pluck-out during polishing being confused with genui

35、ne 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 may become misleading. Secondary phase volume fractions or porosity present at levels o

36、f 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 m

37、ake a reasonable estimate of glassy phase content, the glass material between crystalline grains should be readily observable, 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 a

38、re seldom homogeneous, and the phase contents can vary from micrograph to micrograph. It is essential to survey a sufficiently 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

39、that the selected regions of a prepared cross-section are statistically representative of the whole sampled section.Some users 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 t

40、he scope of this part, but some guidelines are given in Annex A.2 Normative referencesThe following referenced documents are 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

41、 (including any amendments) applies.ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories5EN ISO 13383 2:2016 (E) -DIN EN ISO 13383-2:2016-08 3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1phase volume f

42、ractionvolume occupied by a distinct, identifiable phase present in a material expressed as a fraction of the whole3.2primary phaseprincipal phase within a microstructure, typically comprising more than 50 % by volume or observed area in a cross-section3.3secondary phaseone or more distinct identifi

43、able phases other than a primary crystalline phase in a materialNOTE A secondary phase can be in the form of discrete grains, or as a continuous phase surrounding some or all of the major phase grains. For the purposes of this part of ISO 13383, porosity may be treated as a secondary phase.4 Apparat

44、us4.1 Sectioning equipmentAny suitable method may be used for preparing the test section from the item under investigation. If a diamond-bladed cut-off saw is employed, it is recommended that the grit size should not exceed 150 m.NOTE This grit size is designated as D151 according to ISO 6106 5.4.2

45、Mounting equipmentSuitable metallurgical mounting equipment and media for providing firm gripping of the test piece for polishing.4.3 Grinding and polishing equipmentSuitable grinding and polishing equipment, employing diamond abrasive media.NOTE A sequence of abrasives and techniques recommended fo

46、r polishing are given in Annex A of ISO 13383-1:2012.4.4 MicroscopeAn optical or scanning electron microscope with photomicrographic facilities.NOTE Although the true magnification of the image is unimportant for making the measurement of the volume fraction, it is advised that a reference graticule

47、 may be used to determine magnification in an optical microscope, or a reference grid or latex spheres may be used for calibration of magnification in a scanning electron microscope, and as a check on the homogeneity of magnification across the field of view.An optical microscope is additionally req

48、uired for assessing the quality of polishing (see 5.4).4.5 Transparent gridTransparent square grid on, e.g. acetate film, and with line thickness not exceeding 0,1 mm.NOTE 1 The grid spacing selected is not critical, but may conveniently be between 3 mm and 15 mm to minimize eyestrain. However, it i

49、s necessary that consideration of the requirements of 6.3 is taken into account.6EN ISO 13383 2:2016 (E) -DIN EN ISO 13383-2:2016-08 NOTE 2 A suitable grid may be prepared as a computer plot with sufficient accuracy of line spacing for the purposes of this part of ISO 13383.5 Test piece preparation5.1 SamplingThe test pieces shall be sampled in a manner subject to agreement between parties.NOTE Guidance on this issue may be found in EN 1006 (see Bibliography