DIN EN ISO 4499-2-2010 Hardmetals - Metallographic determination of microstructure - Part 2 Measurement of WC grain size (ISO 4499-2 2008) German version EN ISO 4499-2 2010《硬质合金 显微.pdf

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1、October 2010 Translation by DIN-Sprachendienst.English price group 13No 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).IC

2、S 77.040.99; 77.160!$kTk“1724972www.din.deDDIN EN ISO 4499-2Hardmetals Metallographic determination of microstructure Part 2: Measurement of WC grain size (ISO 4499-2:2008)English translation of DIN EN ISO 4499-2:2010-10Hartmetalle Metallographische Bestimmung der Mikrostruktur Teil 2: Messung der W

3、C Korngre (ISO 4499-2:2008)Englische bersetzung von DIN EN ISO 4499-2:2010-10Mtaux-durs Dtermination mtallographique de la microstructure Partie 2: Mesurage de la taille des grains de WC (ISO 4499-2:2008)Traduction anglaise de DIN EN ISO 4499-2:2010-10Together with DIN EN ISO4499-1:2010-10,supersede

4、sDIN ISO 4499:1991-07www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 24 pages10.10 DIN EN ISO 4499-2:2010-10 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 119 “P

5、owder metallurgy” (Secretariat: SIS, Sweden) in collaboration with Technical Committee CEN/SS M11 “Powder metallurgy” (Secretariat: CCMC). The responsible German body involved in its preparation was the Normenausschuss Werkstofftechnologie (Technology of Materials Standards Committee), Working Commi

6、ttee NA 145-01-04 AA Probenahme und Prfverfahren fr Hartmetalle. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3326 DIN ISO 3326 ISO 3369 DIN EN ISO 3369 ISO 3738-1 DIN EN ISO 3738-1 ISO 3738-2 DIN EN ISO 3738-2 ISO 3878 DIN ISO 3878

7、ISO 4489:1978-06 DIN ISO 4489:1991-07 ISO 4499-1 DIN EN ISO 4499-1 ISO 4505 DIN ISO 4505 Amendments This standard differs from DIN ISO 4499:1991-07 as follows: a) specifications relating to the measurement of WC grain size of hardmetals have been included. Previous editions DIN ISO 4499: 1991-07 DIN

8、 EN ISO 4499-2:2010-10 3 National Annex NA (informative) Bibliography DIN ISO 3326, Hardmetals Determination of (the magnetization) coercivity DIN EN ISO 3369, Impermeable sintered metal materials and hardmetals Determination of density DIN EN ISO 3738-1, Hardmetals Rockwell hardness test (scale A)

9、Part 1: Test method DIN EN ISO 3738-2, Hardmetals Rockwell hardness test (scale A) Part 2: Preparation and calibration of standard test blocks DIN ISO 3878, Hardmetals Vickers hardness test DIN ISO 4489:1991-07, Sintered hardmetals Sampling and testing DIN EN ISO 4499-1, Hardmetals Metallographic de

10、termination of microstructure Part 1: Photomicro-graphs and description DIN ISO 4505, Hardmetals Metallographic determination of porosity and uncombined carbon DIN EN ISO 4499-2:2010-10 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4499-2 May 2010 ICS 77

11、.040.99; 77.160 Supersedes EN 24499:1993English Version Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2008) Mtaux-durs - Dtermination mtallographique de la microstructure - Partie 2: Mesurage de la taille des grains de WC (ISO 4499-2:2

12、008) Hartmetalle - Metallographische Bestimmung der This European Standard was approved by CEN on 30 April 2010. 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 al

13、teration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN 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 t

14、ranslation under the responsibility of a CEN member into its own language and notified to the CEN 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, F

15、rance, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE

16、 FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4499-2:2010: E(ISO 4499-2:2008) Mikrostruktur - Teil 2: Messung der WC Korngre 2 DIN EN ISO 4499-2:2010-10 EN

17、 ISO 4499-2:2010 (E) Contents Page Foreword3 1 Scope 4 2 Normative references 5 3 Terms, definitions, abbreviations, symbols and units.5 4 General information.7 5 Apparatus .8 6 Calibration 9 7 Grain-size measurement by the linear-intercept method 9 8 Reporting. 12 Annex A (informative) Measurement

18、case study 14 Annex B (informative) Report proforma. 18 Bibliography. 20 3 Foreword The text of ISO 4499-2:2008 has been prepared by Technical Committee ISO/TC 119 “Powder metallurgy” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 4499-2:2010. This Euro

19、pean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2010, and conflicting national standards shall be withdrawn at the latest by November 2010. Attention is drawn to the possibility that some of the e

20、lements 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 24499:1993. ISO 4499-2, together with ISO 4499-1, cancels and replaces ISO 4499:1978, which has been technically r

21、evised. A new section has been added for the quantitative measurement of the WC grain size of hardmetals. ISO 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 gr

22、ain size 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, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland

23、, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 4499-2:2008 has been approved by CEN as a EN ISO 4499-2:2010 without any modification. DIN

24、 EN ISO 4499-2:2010-10 EN ISO 4499-2:2010 (E) 1 Scope This part of ISO 4499 gives guidelines for the measurement of hardmetal grain size by metallographic techniques only using optical or electron microscopy. It is intended for sintered WC/Co hardmetals (also called cemented carbides or cermets) con

25、taining primarily WC as the hard phase. It is also intended for measuring the grain size and distribution by the linear-intercept technique. This part of ISO 4499 essentially covers four main topics: calibration of microscopes, to underpin the accuracy of measurements; linear analysis techniques, to

26、 acquire sufficient statistically meaningful data; analysis methods, to calculate representative average values; reporting, to comply with modern quality requirements. The part of ISO 4499 is supported by a measurement case study to illustrate the recommended techniques (see Annex A). The part of IS

27、O 4499 is not intended for the following. Measurements of size distribution. Recommendations on shape measurements. Further research is needed before recommendations for shape measurement can be given. Measurements of coercivity are sometimes used for grain-size measurement, but this current guide i

28、s concerned only with a metallographic measurement method. It is also written for sintered hardmetals and not for characterising powders. However, the method could, in principle, be used for measuring the average size of powders that are suitably mounted and sectioned. DIN EN ISO 4499-2:2010-10 EN I

29、SO 4499-2:2010 (E) 42 Normative references The 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 (including any amendments) applies. ISO 33

30、26, Hardmetals Determination of (the magnetization) coercivity ISO 3369, Impermeable sintered metal materials and hardmetals Determination of density ISO 3738-1, Hardmetals Rockwell hardness test (scale A) Part 1: Test method ISO 3738-2, Hardmetals Rockwell hardness test (scale A) Part 2: Preparatio

31、n and calibration of standard test blocks ISO 3878, Hardmetals Vickers hardness test ISO 4489:1978, Sintered hardmetals Sampling and testing ISO 4499-1, Hardmetals Metallographic determination of microstructure Part 1: Photomicrographs and description ISO 4505, Hardmetals Metallographic determinatio

32、n of porosity and uncombined carbon 3 Terms, definitions, abbreviations, symbols and units 3.1 General A very wide range of terms are used to describe powders or sintered hardmetals of different sizes. For example, the following have been used in a variety of publications and reports. Extra coarse F

33、ine Microfine Coarse Very fine Micrograin Coarse/Medium Ultra fine Nanophase Medium Extr fine Nanograin Medium/Fine Submicron Super fine None of these terms have commonly agreed or well-defined size ranges among users and producers of powders or sintered products. Consequently, following discussion

34、in the hardmetal community, the following terms for the sizes defined in 3.2 are recommended. The uncertainty associated with the measurement of linear-intercept grain size is about 10 %, if typically 200 grains to 300 grains are counted. Thus, measurements on or close to the class boundaries should

35、 be treated carefully. It is recommended that measurements that fall within 10 % of any of the class boundaries should be classed as follows: EXAMPLE 0,19 m as Nano/Ultrafine 0,21 m as Ultrafine/Nano 0,75 m as Submicron/Fine 0,85 m as Fine/Submicron 1,29 m as Fine/Medium 1,31 m as Medium/Fine 2,4 m

36、as Medium/Coarse 2,6 m as Coarse/Medium DIN EN ISO 4499-2:2010-10 EN ISO 4499-2:2010 (E) 53.2 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.2.1 nano with WC grain size 6,0 m NOTE Measured by the mean-linear-intercept method described in this pa

37、rt of ISO 4499. 3.3 Symbols, abbreviations and units For the purposes of this document, the following symbols, abbreviations and units apply. A is the area, in square millimetres (mm)2 wcd is the arithmetic mean linear intercept of WC grains, in micrometres (m) ECD is the equivalent circle diameter,

38、 in millimetres (mm) L is the line length, in millimetres (mm) DIN EN ISO 4499-2:2010-10 EN ISO 4499-2:2010 (E) 6LI is the arithmetic mean-linear-intercept distance, in micrometres (m) il is the measured length of individual intercepts, in micrometres (m) ilis the sum of the measured length of each

39、individual intercept N is the number of grain boundaries traversed n is the number of WC grains intercepted m is the magnification maxm is the maximum magnification minm is the minimum magnification ms is the measured size, in millimetres (mm) as is the actual size, in millimetres (mm) 4 General inf

40、ormation This part of ISO 4499 addresses the issue of good practice for the measurement of a mean value for WC grain size. It recommends the use of a linear-intercept technique for obtaining data. The measurements shall be made using good practice for the preparation of suitable microstructures for

41、examination outlined in ISO 4499-1. The properties and performance of hardmetals are directly dependent on the microstructure developed during manufacture, which in turn is controlled by the character of the starting powder batch. Understanding the microstructure is the key to controlling or improvi

42、ng properties, and therefore the measurement of micro-structural features, particularly grain size and size distribution, is of paramount importance. Methods of metallographic preparation and etching techniques are as important as the grain-size measure-ment method (see 1 to 4 in the Bibliography),

43、and are included in ISO 4499-1. The principal type of hardmetal considered is WC with a Co binder. However, the procedure can be used for hardmetals that contain cubic carbides or which are based on TiC or Ti(C,N). The most direct way to measure the WC grain size is to polish and etch a cross-sectio

44、n of the microstructure and then to use quantitative metallographic techniques to measure a mean value for the grain size, either by area counting or by linear-intercept techniques. There are three ways by which the mean size by number of the WC grains can be defined: by length (of a line across a 2

45、D section of a grain); by area (of 2D sections of grains); by volume (of individual grains). 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 pa

46、rameter counted. DIN EN ISO 4499-2:2010-10 EN ISO 4499-2:2010 (E) 7The value most used to date has been a length parameter. This can be obtained in several ways, for example, by parallel lines or circles as described in ASTM E11212: by linear intercept, called the Heyn method, from a straight line d

47、rawn across the structure; by the equivalent circle diameter1); this is obtained by measuring grain areas and then taking the diameter of a circle of equivalent area. An additional method is that established by Jefferies, where the number of grains per unit area can be counted. This can, if required

48、, be converted to an equivalent circle diameter. It shall be noted that point/area counting provides no information on distribution, and the Jefferies method is not intended for use on multiphase materials such as hardmetals. The recommended technique for measurement of hardmetal grain size is the l

49、inear-intercept method. 5 Apparatus Grain-size measurements are obtained from images of the microstructure. ISO 4499-1, ASTM B657 10and ASTM B665 11 should be consulted for best practice in the preparation of surfaces for imaging. Hardmetal structural images are usually generated by either optical microscopy or scanning electron microscopy (SEM). For accurate measurements, it is better to use scanning electron-microscopic images. Even in coarse-grained material