1、BSI Standards PublicationBS EN ISO 4499-3:2016Hardmetals Metallographicdetermination ofmicrostructurePart 3: Measurement of microstructuralfeatures in Ti (C, N) and WC/cubic carbidebased hardmetalsBS EN ISO 4499-3:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation o
2、f EN ISO 4499-3:2016.The UK participation in its preparation was entrusted to Technical Committee ISE/65, Sintered metal components.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 provisi
3、ons of a contract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 77836 0 ICS 77.040.99; 77.160 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was
4、published under the authority of the Standards Policy and Strategy Committee on 31 March 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4499-3 March 2016 ICS 77.040.99; 77.160 English Version Hardmetals - Metall
5、ographic determination of microstructure - Part 3: Measurement of microstructural features in Ti (C, N) and WC/cubic carbide based hardmetals (ISO 4499-3:2016) Mtaux-durs - Dtermination mtallographique de la microstructure - Partie 3: Mesure des caractristiques des microstructures des mtaux-durs bas
6、e de carbures Ti (C, N) et WC/cubiques (ISO 4499-3:2016)Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 3: Messung von mikrostrukturellen Merkmalen in Hartmetallen auf Basis von Ti (C, N) und WC/kubischem Carbid (ISO 4499-3:2016) This European Standard was approved by CEN on 4 Fe
7、bruary 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 lists and bibliographical references concerning such national standards may be
8、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 the responsibility of a CEN member into its own language and notified to th
9、e 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 Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ire
10、land, Italy, Latvia, Lithuania, Luxembourg, 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 Cen
11、tre: 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 4499-3:2016 EBS EN ISO 4499-3:2016EN ISO 4499-3:2016 (E) 3 European foreword This document (EN ISO 4499-3:2016) has been prepared by Te
12、chnical Committee ISO/TC 119 “Powder metallurgy“. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2016, and conflicting national standards shall be withdrawn at the latest by September 2
13、016. 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 not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organiz
14、ations of the following countries are bound to implement this European 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, Ma
15、lta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 4499-3:2016 has been approved by CEN as EN ISO 4499-3:2016 without any modification. BS EN ISO 4499-3:2016ISO 4499-3:2016(E)Foreword
16、ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols and units . 25 Principle 36 Apparatus . 37 Calibration 48 Preparation of test samples 48.1 Metallographic preparation . 48.2 Ti(C, N) based hardmetals cermets. 48.3 WC/Cubic carbide based hardmetals 89 Procedure
17、for characterisation of structures209.1 Sampling of images of structure . 209.1.1 General. 209.1.2 Representative selection 209.1.3 Determination of homogeneity of hard phase sizes .209.1.4 Inhomogeneous materials 219.2 Phase size measurement . 219.2.1 General. 219.2.2 Phase measurement by intercept
18、s 2110 Uncertainty of measurement 2311 Test report 23Bibliography .25 ISO 2016 All rights reserved iiiContents PageBS EN ISO 4499-3:2016ISO 4499-3:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The w
19、ork 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 organizations, governmental and non-govern
20、mental, 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.The procedures used to develop this document and those intended for its further maintenance are described in t
21、he ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the poss
22、ibility 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. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list o
23、f patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as
24、information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information.The committee responsible for this document is ISO/TC 119, Powder metallurgy, Subcommittee SC 4, Sampling and testing methods for hardmetals.ISO
25、 4499 consists of the following parts, under the general title Hardmetals Metallographic determination of microstructure: Part 1: Photomicrographs and description Part 2: Measurement of WC grain size Part 3: Measurement of microstructural features in Ti(C,N) and WC/cubic carbide based hardmetals Par
26、t 4: Characterisation of porosity, carbon defects and eta-phase contentiv ISO 2016 All rights reservedBS EN ISO 4499-3:2016ISO 4499-3:2016(E)IntroductionThis part of ISO 4499 essentially covers the following topics: materials types and phases to be measured including the following: Ti(C, N) cermets;
27、 WC/Cubic carbide hardmetals; preparation methods to highlight differences between conventional WC/Co hardmetals and materials containing cubic phases; linear analysis techniques to acquire sufficient statistically meaningful data for phase quantification; analysis method to calculate representative
28、 average values; reporting to comply with modern quality requirements. ISO 2016 All rights reserved vBS EN ISO 4499-3:2016BS EN ISO 4499-3:2016Hardmetals Metallographic determination of microstructure Part 3: Measurement of microstructural features in Ti (C, N) and WC/cubic carbide based hardmetals1
29、 ScopeThis part of ISO 4499 gives guidelines for the measurement of microstructural features in Ti(C,N) based hardmetals and WC/Co hardmetals that contain additional cubic carbides by metallographic techniques only using optical or electron microscopy. It is intended for sintered hardmetals (also ca
30、lled cemented carbides or cermets) containing primarily inorganic carbides and nitrides as the hard phase. It is also intended for measuring the phase size and distribution by the linear intercept technique.2 Normative referencesThe following documents, in whole or in part, are normatively reference
31、d in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 44991:2008, Hardmetals Metallographic determination of microstructure Part
32、1: Photomicrographs and descriptionISO 44992:2008, Hardmetals Metallographic determination of microstructure Part 2: Measurement of WC grain size3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1nanowith carbonitride or cubic carbide phase size 6,
33、0 m, respectivelyNote 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.3.8Ti(C, N) cermetsTiCN-based cermet contains 3 to 30 weight % of a binder phase mainly composed of Co and/or Ni, but may also include MoNote 1 to entry: The balance being substantially a hard phas
34、e and a few minor impurities.Note 2 to entry: The hard phase is mainly composed of titanium carbide, nitride and/or carbonitride, but may also include carbonitrides of (Ti,Ta), (Ti,W) or (Ti,Ta, W). Note 3 to entry: These materials typically contain hard phases that can have grains with a core/rim s
35、tructure.3.9WC/Cubic carbide hardmetalshexagonal WC-based hardmetals containing substantial amounts of a carbide having a cubic lattice, such as, for example TiC or TaC, and which can contain W in solid solutionNote 1 to entry: These materials typically contain hard phases that may have grains with
36、a core/rim structure.Note 2 to entry: See Table 1.3.10phase regionsingle constituent of the hardmetal like WC, cubic carbide or binder4 Symbols and unitsA area, in square millimetres (mm2) ECD Equivalent Circle Diameter of a specified phase, in micrometres (m)L total line length in a specified phase
37、, in millimetres (mm)limeasured length of individual intercepts in a specified phase, in micrometres (m)lisum of the measured length of each individual intercept2 ISO 2016 All rights reservedBS EN ISO 4499-3:2016ISO 4499-3:2016(E)lxarithmetic mean linear intercept in phase x, in micrometres (m)N num
38、ber of grain boundaries traversed in or between specified phasesn number of WC, carbonitride or cubic carbide grains interceptedm magnificationmmaxmaximum magnificationmminminimum magnification5 PrincipleThis part of ISO 4499 addresses the issue of good practice for the measurement of a mean value f
39、or the hard phase and binder phase size in hardmetals other than straight WC/Co. It recommends the use of a linear intercept technique for obtaining data on feature sizes. The measurements are to be made using good practice for the preparation of suitable microstructures for examination outlined in
40、ISO 4499-1.Methods of metallographic preparation and etching techniques are as important as the phase size measurement method (see also ASTM B 657, ASTM B 665, Reference 1 and Reference 2). Basic methods are described in ISO 4499-1. Further relevant information is given in Clause 8. The principal ty
41、pes of hardmetal considered are those that contain cubic carbides as well as WC and those that are based on TiC or Ti(C,N).345A cubic carbide phase is defined as a carbide having a cubic lattice, such as, for example, TiC or TaC, and which usually also contains W in solid solution after sintering. T
42、hese materials typically contain hard phases that have grains with a core/rim structure. Guidelines to measure these internal details are included in ISO 44992:2008, Annex A.The most direct way to measure the phase size is to polish and etch a cross-section of the microstructure and then to use quan
43、titative metallographic techniques to measure a mean value for the feature size, either by area counting or by linear intercept techniques.The following are three ways by which the mean size by number of the various phases can be defined: by length (of a line across a 2D section of a phase); by area
44、 (of 2D sections of phase regions); by volume (of individual phase regions).A number average is obtained by counting each measurement of the parameter of interest (length, area or volume) and dividing the total value of the parameter (length, area or volume) by the number of this parameter counted.T
45、he values for phase size most used to date have been based on a length parameter. This can be obtained in the following several ways, for example: by parallel lines or circles as described in ASTM E112; by linear intercept, called the Heyn method, from a straight line drawn across the structure; by
46、equivalent circle diameter (see ISO 4499-2), this is obtained by measuring hard phase grain areas and then taking the diameter of a circle of equivalent area.6 Apparatus6.1 Metallographic optical microscope, or other suitable equipment permitting observations and measurements on a screen up to the r
47、equired magnification. ISO 2016 All rights reserved 3BS EN ISO 4499-3:2016ISO 4499-3:2016(E)6.2 Scanning electron microscope, permitting observations and measurements of features too small to be resolved with an optical microscope.6.3 Equipment for preparation of test-piece sections.Phase size measu
48、rements are obtained from images of the microstructure. ISO 4499-1, ASTM B 657 and ASTM B 665 should be consulted for best practice in the preparation of surfaces for imaging.Structural images are usually generated by either optical microscopy or Scanning Electron Microscopy (SEM). For accurate meas
49、urements, it is better to use scanning electron microscopic images. Even in coarse grained materials, the imaged surface cuts through a substantial number of the corners of grains giving a proportion of small intercepts that can only be measured accurately using the scanning electron microscope.Measurements of intercept lengths from the acquired images can be obtained manually or semi-automatically using image analysis. Automatic image analysis can be used in some circumstances when the images are fairly c
