DIN EN ISO 4499-4-2016 Hardmetals - Metallographic determination of microstructure - Part 4 Characterisation of porosity carbon defects and eta-phase content (ISO 4499-4 2016) Germ.pdf

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1、October 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 77.040.99; 77.160!%n?“2577528www

2、.din.deDIN EN ISO 4499-4Hardmetals Metallographic determination of microstructure Part 4: Characterisation of porosity, carbon defects and etaphase content (ISO 44994:2016);English version EN ISO 44994:2016,English translation of DIN EN ISO 4499-4:2016-10Hartmetalle Metallographische Bestimmung der

3、Mikrostruktur Teil 4: Charakterisierung von Porositt, Kohlenstofffehlern und Anteil an EtaPhase (ISO 44994:2016);Englische Fassung EN ISO 44994:2016,Englische bersetzung von DIN EN ISO 4499-4:2016-10Mtauxdurs Dtermination mtallographique de la microstructure Partie 4: Caractrisation de la porosit, d

4、es dfauts carbone et de la teneur en phase ta (ISO 44994:2016);Version anglaise EN ISO 44994:2016,Traduction anglaise de DIN EN ISO 4499-4:2016-10SupersedesDIN ISO 4505:199107www.beuth.deDocument comprises 19 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shal

5、l be considered authoritative.09.16 DIN EN ISO 4499-4:2016-10 2 A comma is used as the decimal marker. National foreword This document (EN ISO 4499-4:2016) has been prepared by Technical Committee ISO/TC 119 “Powder metallurgy”, Subcommittee SC 4 “Sampling and testing methods for hardmetals”. The re

6、sponsible German body involved in its preparation was DIN-Normenausschuss Werkstofftechnologie (DIN Standards Committee Technology of Materials), Working Committee NA 145-01-04 AA Probenahme und Prfverfahren fr Hartmetalle. In addition to the SEM (scanning electron microscope) named in this standard

7、, the use of an FESEM (field emission scanning electron microscope) is also recommended. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 4499-2:2008 DIN EN ISO 4499-2:2010-10 Amendments This standard differs from DIN ISO 4505:1991-07 as fo

8、llows: a) the title of the standard has been modified; b) Clause 2 “Normative references”, Clause 3 “Terms and definitions”, Clause 4 “Symbols and units”, Clause 5 “Principle”, Subclause 6.2 “Scanning electron microscope”, Clause 7 “Calibration of measurement apparatus”, Subclause 8.2 “Characterisat

9、ion of porosity and carbon (graphite) defects” and Subclause 8.3 “Characterisation of eta-phase” have been added; c) Subclause 9.4 “Determination of the -phase (eta phase)” has been added, including Figure 5 “Large eta-phase rosettes (about 100 m in diameter)” and Figure 6 “Small eta-phase particles

10、 (light grey, about 5 m in diameter)”; d) Clause 10 “Uncertainty of measurement has been added; e) Clause 11 “Test report” has been expanded; f) the standard has been editorially revised. Previous editions DIN ISO 4505: 1991-07 DIN EN ISO 4499-4:2016-10 3 National Annex NA (informative) Bibliography

11、 DIN EN ISO 4499-2:2010-10, Hardmetals Metallographic determination of microstructure Part 2: Measurement of WC grain size (ISO 4499-2:2008) DIN EN ISO 4499-4:2016-10 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4499-4 March 2016 ICS 77.040.99; 77.160 S

12、upersedes EN 24505:1993English Version Hardmetals - Metallographic determination of microstructure - Part 4: Characterisation of porosity, carbon defects and eta-phase content (ISO 4499-4:2016)Mtaux-durs - Dtermination mtallographique de la microstructure - Partie 4: Caractrisation de la porosit, de

13、s dfauts carbone et de la teneur en phase ta (ISO 4499-4:2016) Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 4: Charakterisierung von Porositt, Kohlenstofffehlern und Anteil an Eta-Phase (ISO 4499-4:2016) This European Standard was approved by CEN on 4 February 2016. CEN member

14、s 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 obtained on application

15、 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 the CEN-CENELEC Managemen

16、t 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, Ireland, Italy, Latvia, Li

17、thuania, 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 Centre: Avenue Marnix 17,

18、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 4499-4:2016 EForeword 4Introduction 51 Scope .62 Normative references 63 Terms and definitions .64 Symbols and Units .65 Principle 76 Apparatus .77 Calibratio

19、n of measurement apparatus .78 Preparation of test samples 78.1 Methods of preparation .78.2 Characterisation of porosity and carbon (graphite) defects .88.3 Characterisation of eta-phase 89 Procedure.89.1 General .89.2 Determination of porosity .89.3 Determination of carbon defects .99.4 Determinat

20、ion of the -phase (eta-phase).1210 Uncertainty of measurement 1411 Test report 14Bibliography .15Contents PageEN ISO 4499-4:2016 (E) DIN EN ISO 4499-4:2016-10 2European foreword .3European foreword This document (EN ISO 4499-4:2016) has been prepared by Technical Committee ISO/TC 119 Powder metallur

21、gy . 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 2016. Attention is drawn to the possibility th

22、at 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. This document supersedes EN 24505:1993. According to the CEN-CENELEC Internal Regulations, the national standards organization

23、s 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, Malta,

24、Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 4499-4:2016 has been approved by CEN as EN ISO 4499-4:2016 without any modification. EN ISO 4499-4:2016 (E) DIN EN ISO 4499-4:2016-10 3“”F

25、orewordISO (the International Organization for Standardization) 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 tec

26、hnical 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 part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters o

27、f electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document

28、 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 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 p

29、atent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of 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 no

30、t constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information

31、.The committee responsible for this document is ISO/TC 119, Powder metallurgy, Subcommittee SC 4, Sampling and testing methods for hardmetals.This first edition of ISO 4499-4 cancels and replaces ISO 4505:1978, which has been technically revised.ISO 4499 consists of the following parts, under the ge

32、neral 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 Part 4: Characterisation of porosity, carbon defects

33、and eta-phase contentEN ISO 4499-4:2016 (E) DIN EN ISO 4499-4:2016-10 4 IntroductionIn standard WC/Co hardmetals, the chemistry, magnetic properties and density are generally controlled so that only two phases WC and Co are present.123The Co phase is an alloy and contains some W and C in solid solut

34、ion. The WC phase is stoichiometric. If the composition is either high or low in total carbon content, then it is possible to see a third phase in the structure. For high C, this is graphite; for low C, it is eta phase (); typically, an M6C or M12C carbide where M is (CoxWy). This part of ISO 4499 i

35、s concerned with the detection and measurement of these microstructural features together with the measurement of porosity levels. Porosity is important since these materials are manufactured by a powder metallurgical route and although the technique of liquid phase sintering is used to consolidate

36、the multiphase structure, low levels of porosity can arise in some instances and affect properties such as density and strength.EN ISO 4499-4:2016 (E) DIN EN ISO 4499-4:2016-10 5 1 ScopeThis part of ISO 4499 specifies methods for the metallographic determination of the presence, type, and distributi

37、on of porosity, uncombined carbon and eta-phase in hardmetals.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the l

38、atest edition of the referenced document (including any amendments) applies.ISO 4499-2:2008, 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.3.1carbon def

39、ectsmacroscopic precipitates of carbon (graphite) which can be in the form of large angular rosettes or small flakes3.2eta-phase-phasecubic carbide based on M6C or M12C structure where M is a mixture of Co and W usually in equal proportions; and which can be present as large (up to 100 m diameter) r

40、osettes or small micrometre-sized particles4 Symbols and UnitsECD Equivalent Circle Diameter of a specified phase, in micrometres (m)L total line length in a specified phase, in millimetres (mm)limeasured length of individual intercepts in a specified phase, in micrometres (m)lisum of the measured l

41、ength of each individual interceptlxarithmetic mean linear intercept in phase x, in micrometres (m)EN ISO 4499-4:2016 (E) DIN EN ISO 4499-4:2016-10 6 N number of eta-phase particles interceptedm magnificationmmaxmaximum magnificationmminminimum magnification5 PrincipleThis part of ISO 4499 handles t

42、he following key issues: description of methods for sample preparation; description of how to identify and measure the relevant feature.In some cases, the approach adopted in ISO 4499-2 and ISO 4499-3 can be useful, whereby the intercept method is used on microphotographs of the structure for releva

43、nt quantification of feature size, such as eta-phase or graphite rosettes.6 Apparatus6.1 Metallographic optical microscope, or other suitable equipment permitting observations and measurements on a screen up to the required magnification.6.2 Scanning electron microscope (SEM), permitting observation

44、s and measurements of features too small to be resolved with an optical microscope.6.3 Equipment for preparation of test-piece sections.7 Calibration of measurement apparatusFor reliable quantitative measurements, images shall be calibrated against a stage micrometre or scale traceable to a National

45、 Reference Standard. The most commonly used stage micrometres for SEMs are the SIRA grids. These are ruled lines which form a grid and are available with 19,7 lines/mm and 2 160 lines/mm. However, these shall also be calibrated and certified as being traceable to a National Reference Standard.For im

46、ages obtained from an optical microscope, an image of the calibration graticule shall also be obtained using the same objectives (and internal magnification step changers or zoom position) and illuminating technique. The microscope shall be set up for Khler illumination to obtain the maximum resolut

47、ion, see Reference 4.For images obtained from a scanning electron microscope, images of the graticule should be obtained under the same conditions (accelerating kV, working distance, illumination aperture) as those used for the hardmetal.8 Preparation of test samples8.1 Methods of preparationThere a

48、re several methods for the preparation of hardmetal surfaces for metallographic examination. For example, a detailed description is given in ISO 4499-1. Firstly, careful coarse grinding is carried out to remove sufficient material to ensure that the true structure is revealed. After grinding with fine diamond grit wheels, polishing is effected by using diamond paste or diamond powders of progressively finer grain size down to 1 m on rigidly supported laps of, for example, thin plastic, t