DIN EN ISO 13383-1-2016 Fine ceramics (advanced ceramics advanced technical ceramics) - Microstructural characterization - Part 1 Determination of grain size and size distribution .pdf

1、November 2016 English price group 14No 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!%u“2588288www.din.deD

2、IN EN ISO 13383-1Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterization Part 1: Determination of grain size and size distribution (ISO 133831:2012);English version EN ISO 133831:2016,English translation of DIN EN ISO 13383-1:2016-11Hochleistungskeramik Mikros

3、trukturelle Charakterisierung Teil 1: Bestimmung der Korngre und der Korngrenverteilung (ISO 133831:2012);Englische Fassung EN ISO 133831:2016,Englische bersetzung von DIN EN ISO 13383-1:2016-11Cramiques techniques Caractrisation microstructurale Partie 1: Dtermination de la taille et de la distribu

4、tion des grains (ISO 133831:2012);Version anglaise EN ISO 133831:2016,Traduction anglaise de DIN EN ISO 13383-1:2016-11SupersedesDIN EN 6233:200301www.beuth.deDocument comprises 29 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritativ

5、e.11.16 DIN EN ISO 13383-1:2016-11 2 A comma is used as the decimal marker. National foreword The text of ISO 13383-1:2012 has been prepared by Technical Committee ISO/TC 206 “Fine ceramics” and has been taken over as EN ISO 13383-1:2016 by Technical Committee CEN/TC 184 “Advanced technical ceramics

6、” (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 Hochleistungskeramik und Prfung von monolithischen keramischen Werkstoffen und

7、 Pulvern. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 6106 DIN ISO 6106 ISO/IEC 17025 DIN EN ISO/IEC 17025 Amendments This standard differs from DIN EN 623-3:2003-01 as follows: a) Subclauses 5.4 “Etching equipment” and 5.7 “Circle

8、template” have been included in Clause 5 “Apparatus”; b) Clause 8 “Measurement of micrographs” has been rendered more precise and method A has been subdivided into method A.1 and method A.2; c) use of a stencil is illustrated in Figure 2 to clarify method B; d) Subclause 9.2 “Method A2” has been new

9、ly added in Clause 9 “Calculation of results”; e) ISO 13383-1:2012 has been adopted. Previous editions DIN V ENV 623-3: 1993-04 DIN EN 623-3: 2003-01 National Annex NA (informative) Bibliography DIN EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories DIN

10、 ISO 6106, Abrasive products Checking the grain size of superabrasives EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13383-1 April 2016 ICS 81.060.30 Supersedes EN 623-3:2001English Version Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural characterization -

11、 Part 1: Determination of grain size and size distribution(ISO 13383-1:2012) Cramiques techniques - Caractrisation microstructurale - Partie 1: Dtermination de la taille et de la distribution des grains (ISO 13383-1:2012) Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 1: Bestimmun

12、g der Korngre und der Korngrenverteilung (ISO 13383-1:2012) This European Standard was approved by CEN on 18 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 withou

13、t any alteration. Up-to-date lists 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 la

14、nguage made by translation under 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, Denm

15、ark, 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, Turkey andUnited Kingdom. EUROPEAN COMMITTEE

16、FOR STANDARDIZATION COMIT EUROPEN 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 13383-1:2016 EContents Page

17、European foreword .31 Scope . 52 Normative references 53 Terms and definitions . 54 Significance and use 75 Apparatus . 85.1 Sectioning equipment . 85.2 Mounting equipment . 85.3 Grinding and polishing equipment 85.4 Etching equipment. 85.5 Microscope . 85.6 Calibrated rule or scale 95.7 Circle temp

18、late 96 Test piece preparation 96.1 Sampling . 96.2 Cutting 96.3 Mounting 96.4 Grinding and polishing . 96.5 Etching 107 Photomicrography . 107.1 General aspects 107.2 Optical microscopy . 107.3 Scanning electron microscopy 107.4 Calibration micrographs 118 Measurement of micrographs 118.1 General 1

19、18.2 Method A1 128.3 Method A2 128.4 Method B . 128.5 Use of automatic or semi-automatic image analysis for methods A and B 139 Calculation of results 149.1 Method A1 149.2 Method A2 149.3 Method B . 1410 Interferences and uncertainties 1511 Test report 16Annex A (informative) Grinding and polishing

20、 procedures 18Annex B (informative) Etching procedures 20Annex C (informative) Setting Khler illumination in an optical microscope .22Annex D (informative) Round-robin verification of Method A123Annex E (informative) Round-robin verification of Method B 24Annex F (informative) Grain size distributio

21、n measurement .25Annex G (informative) Results sheet: Grain size in accordance with ISO 13383-1 .26Bibliography .27DIN EN ISO 13383-1:2016-11 EN ISO 13383-1:2016 (E) 2Foreword .4European foreword The text of ISO 13383-1:2012 has been prepared by Technical Committee ISO/TC 206 “Fine ceramics” of the

22、International Organization for Standardization (ISO) and has been taken over as EN ISO 13383-1:2016 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 publication

23、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 shall n

24、ot be held responsible for identifying any or all such patent rights. This document supersedes EN 623-3:2001. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

25、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, Turkey a

26、nd the United Kingdom. Endorsement notice The text of ISO 13383-1:2012 has been approved by CEN as EN ISO 13383-1:2016 without any modification. DIN EN ISO 13383-1:2016-11 EN ISO 13383-1:2016 (E)3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national

27、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. International

28、 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 rules gi

29、ven 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 least

30、75 % of the member bodies casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 13383-1 was prepared by Technical Committee ISO/TC 206, F

31、ine 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 fraction by evaluation of m

32、icrographsDIN EN ISO 13383-1:2016-11 EN ISO 13383-1:2016 (E) 4 1 ScopeThis part of ISO 13383 describes manual methods of making measurements for the determination of grain size of fine ceramics (advanced ceramics, advanced technical ceramics) using photomicrographs of polished and etched test pieces

33、. The methods described in this part do not yield the true mean grain diameter, but a somewhat smaller parameter depending on the method applied to analyse a two-dimensional section. The relationship to true grain dimensions depends on the grain shape and the degree of microstructural anisotropy. Th

34、is part contains two principal methods, A and B.Method A is the mean linear intercept technique. Method A1 applies to single-phase ceramics, and to ceramics with a principal crystalline phase and a glassy grain-boundary phase of less than about 5 % by volume for which intercept counting suffices. Me

35、thod A2 applies to ceramics with more than about 5 % by volume of pores or secondary phases, or ceramics with more than one major crystalline phase where individual intercept lengths are measured, which can optionally be used to create a size distribution. This latter method allows the pores or phas

36、es to be distinguished and the mean linear intercept size for each to be calculated separately.NOTE A method of determining volume fraction(s) of secondary phase(s) can be found in ISO 13383:2; this will provide a means of determining whether Method A1 or Method A2 should be applied in borderline ca

37、ses.Method B is the mean equivalent circle diameter method, which applies to any type of ceramic with or without a secondary phase. This method may also be employed for determining grain aspect ratio and a size distribution.Some users of this part of ISO 13383 may wish to apply automatic or semiauto

38、matic image analysis to micrographs or directly captured microstructural images. This is permitted by this part provided that the technique employed simulates the manual methods (see Clause 4 and 8.4).2 Normative referencesThe following referenced documents are indispensable for the application of t

39、his 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 laboratories3 Terms and definitionsFor the pu

40、rposes of this document, the following terms and definitions apply.3.1grain sizesize of the distinct crystals in a material, and for the purposes of this method of test, that of the primary or major phaseDIN EN ISO 13383-1:2016-11 EN ISO 13383-1:2016 (E)5 3.2mean linear intercept grain sizegmliavera

41、ge value of the distance between grain boundaries as shown by randomly positioned lines drawn across a micrograph or other image of the microstructure3.3equivalent circle grain diameterdcidiameter of a circle which closely matches the perimeter of a grainSee Figure 1.3.4maximum (Feret) grain sizedci

42、, maxmaximum dimension of a grain viewed in two dimensionsSee Figure 1.NOTE This is also termed maximum caliper diameter in ASTM E930.3.5maximum orthogonal grain sizedci, perpfor the purposes of determination of grain aspect ratio, the largest dimension of a grain normal to its maximum (Feret) grain

43、 dimension, viewed in two dimensionsSee Figure 1.3.6grain aspect ratioratio of maximum (Feret) grain size to the maximum orthogonal grain size measured perpendicular to itDIN EN ISO 13383-1:2016-11 EN ISO 13383-1:2016 (E) 6 132Key1 Equivalent circle grain diameter, dci2 Maximum grain (Feret) size, d

44、ci, max3 Maximum orthogonal grain size perpendicular to 2, dci, perpFigure 1 Equivalent circle diameter and definition of aspect ratio4 Significance and useThe mean grain size and the distribution of grain sizes of a ceramic material play an important role in determining many properties, and thus gr

45、ain size characterization is an important tool for ensuring consistency of manufacture. There are many measures of grain size and/or shape, and these are usually of different numerical values for a given microstructure.NOTE The Bibliography contains sources dealing with stereology and methods of siz

46、ing three-dimensional objects.The principal purpose of this part of ISO 13383 is to permit characterization of the major phases. However, in materials which contain more than one phase, the phases may be continuous or as isolated grains. It may be necessary to characterize the different phases separ

47、ately. The same intercept principle as for single-phase materials can be used, but the individual intercept lengths across each phase must be measured, rather than just counted. The characterization of minor phases may require different treatment, which is outside the scope of this part of ISO 13383

48、.Method A, the linear intercept method, provides the simplest possible method from a two-dimensional section through the material. However, it must be recognized that the numerical value obtained for the mean linear intercept size is somewhat smaller than most other measures of grain size because intercepts can cross grains at any position, and not necessarily along the largest axis. The relationship between mean linear intercept size and a t