SIST EN ISO 4499-2:2010

Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2008)

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) containing 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 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). Measurements of coercivity are sometimes used for grain-size measurement, but this current guide is 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.

Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 2: Messung der WC Korngröße (ISO 4499-2:2008)

Dieser Teil von ISO 4499 gibt Leitlinien für die Messung der Hartmetallkorngröße mittels metallographischer Verfahren ausschließlich unter Anwendung der Licht  oder Elektronenmikroskopie an. Dieser ist für gesinterte WC/Co Hartmetalle (auch als Sinterhartmetalle oder Cermets bezeichnet) vorgesehen, die hauptsächlich WC als harte Phase haben. Er ist ebenfalls für die Messung der Korngröße und deren Verteilung mit dem Linienschnittverfahren vorgesehen.
Dieser Teil von ISO 4499 deckt im Wesentlichen vier Hauptthemen ab:
-   Kalibrierung von Mikroskopen zur Steigerung der Messgenauigkeit;
-   lineare Analysenverfahren zum Erhalten von statistisch aussagekräftigen Daten;
-   Analysenverfahren zur Berechnung von repräsentativen Mittelwerten;
-   Auswertung entsprechend den gegenwärtigen Qualitätsanforderungen.
In diesem Teil von ISO 4499 werden die empfohlenen Verfahren durch eine (messtechnische) Fallstudie (siehe Anhang A) veranschaulicht.
Dieser Teil von ISO 4499 ist nicht für Folgendes vorgesehen:
-   Messungen von Korngrößenverteilung;
-   Empfehlungen für Formmessungen. Weitere Untersuchungen sind erforderlich, bevor Empfehlungen für Formmessung gegeben werden können.
Zur Messung der Korngröße werden mitunter Messungen von Koerzitiv-Feldstärke herangezogen, der vor-liegende Leitfaden befasst sich jedoch ausschließlich mit einem metallographischen Messverfahren. Darüber hinaus ist er für gesinterte Hartmetalle und nicht zur Charakterisierung von Pulvern vorgesehen. Das Verfahren kann jedoch grundsätzlich zur Messung der mittleren Korngröße von Pulvern, die in geeigneter Weise eingebettet und geteilt sind, herangezogen werden.

Métaux-durs - Détermination métallographique de la microstructure - Partie 2: Mesurage de la taille des grains de WC (ISO 4499-2:2008)

L'ISO 4499-2:2008 donne des lignes directrices relatives au mesurage de la taille des grains de métaux‑durs selon des techniques métallographiques utilisant uniquement un microscope optique ou électronique. Elle est destinée aux métaux‑durs WC/Co frittés (également appelés carbures cémentés ou cermets) contenant principalement du WC sous la forme d'une phase dure. Elle est également destinée au mesurage de la taille des grains et de la distribution au moyen de la technique d'interception linéaire.
L'ISO 4499-2:2008 couvre essentiellement quatre sujets principaux:
étalonnage de microscopes, pour appuyer la précision des mesures;
techniques d'analyses linéaires, pour obtenir suffisamment de données statistiquement significatives;
méthodes d'analyse, pour calculer des valeurs moyennes représentatives;
rapports, pour répondre aux exigences modernes de qualité.
L'ISO 4499-2:2008 ne traite pas les points suivants.
mesurages de la distribution des grains;
recommandations sur les mesurages de forme. De plus amples recherches sont nécessaires avant de pouvoir établir des recommandations relatives au mesurage de forme.
Des mesurages de coercivité servent parfois au mesurage de la taille des grains, toutefois les lignes directrices données ici ne traitent que de la méthode de mesurage métallographique. L'ISO 4499-2:2008 est également rédigée pour les métaux‑durs frittés et non pour les poudres caractérisantes. Toutefois, la méthode peut, en principe, servir au mesurage de la granulométrie moyenne de poudres convenablement montées et sectionnées.

Trdine - Metalografsko določevanje mikrostrukture - 2. del: Merjenje velikosti zrn volframovega karbida (WC) (ISO 4499-2:2008)

Ta del ISO 4499 podaja smernice za merjenje velikosti zrna trdin z metalografskimi tehnikami, ki uporabljajo samo optično ali elektronsko mikroskopiranje. Namenjen je za sintrane WC/CO trdine (prav tako imenovane cementirani karbidi ali cermet), ki vsebujejo predvsem volframov karbid v trdni fazi. Prav tako je namenjen za merjenje velikosti zrn in distribucijo s tehniko linearnega prestrezanja. Ta del ISO 4499 predvsem zajema štiri glavne teme: - kalibracijo mikroskopov za podpiranje natančnosti merjenj; - linearne analizne tehnike za doseganje zadostnih statistično pomembnih podatkov; - analizne metode za izračun reprezentativnih povprečnih vrednostih; - poročanje za skladnost z modernimi zahtevami glede kakovosti.  Ta del ISO 4499 je podprt s študijo primera merjenja, ki ponazarja za priporočene tehnike (glej Dodatek A). Včasih se za merjenje velikosti zrn uporabijo meritve koercitivnosti, vendar to pričujoče vodilo zadeva samo metode metalografskega merjenja. Prav tako je napisano za sintrane trdine in ne za lastnosti praškov. Vendar se načeloma metoda lahko uporabi za merjenje povprečne velikosti praškov, ki so ustrezno kopičeni in razdeljeni.

General Information

• Status: Withdrawn
• Public Enquiry End Date: 04-Feb-2010
• Publication Date: 18-May-2010
• Withdrawal Date: 12-Aug-2020
• ICS: 77.040.99 - Other methods of testing of metals
• ICS: 77.160 - Powder metallurgy
• Technical Committee: I13 - Imaginarni 13
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 13-Aug-2020
• Due Date: 05-Sep-2020
• Completion Date: 13-Aug-2020
• Ref Project: EN ISO 4499-2:2010 - Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2008)

Relations

• Replaced By: SIST EN ISO 4499-2:2020 - Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2020)
• Effective Date: 12-Aug-2020
• Replaces: SIST EN 24499:2000 - Hardmetals - Metallographic determination of microstructure (ISO 4499:1978)
• Effective Date: 01-Jul-2010
• Revised: SIST EN ISO 4499-2:2020 - Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2020)
• Effective Date: 13-Nov-2017
• Replaces: SIST EN 24499:2000 - Hardmetals - Metallographic determination of microstructure (ISO 4499:1978)
• Effective Date: 08-Jun-2022

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 4499-2:2010
01-julij-2010
1DGRPHãþD
SIST EN 24499:2000
7UGLQH0HWDORJUDIVNRGRORþHYDQMHPLNURVWUXNWXUHGHO0HUMHQMHYHOLNRVWL]UQ
YROIUDPRYHJDNDUELGD:&,62
Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of
WC grain size (ISO 4499-2:2008)
Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 2: Messung der WC
Korngröße (ISO 4499-2:2008)
Métaux-durs - Détermination métallographique de la microstructure - Partie 2: Mesurage
de la taille des grains de WC (ISO 4499-2:2008)
Ta slovenski standard je istoveten z: EN ISO 4499-2:2010
ICS:
77.040.99 Druge metode za Other methods of testing of
preskušanje kovin metals
77.160 Metalurgija prahov Powder metallurgy
SIST EN ISO 4499-2:2010 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 4499-2:2010

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SIST EN ISO 4499-2:2010


EUROPEAN STANDARD
EN ISO 4499-2

NORME EUROPÉENNE

EUROPÄISCHE NORM
May 2010
ICS 77.040.99; 77.160 Supersedes EN 24499:1993
English Version
Hardmetals - Metallographic determination of microstructure -
Part 2: Measurement of WC grain size (ISO 4499-2:2008)
Métaux-durs - Détermination métallographique de la Hartmetalle - Metallographische Bestimmung der
microstructure - Partie 2: Mesurage de la taille des grains Mikrostruktur - Teil 2: Messung der WC Korngröße (ISO
de WC (ISO 4499-2:2008) 4499-2:2008)
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 alteration. 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 translation
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, France, 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
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4499-2:2010: E
worldwide for CEN national Members.

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SIST EN ISO 4499-2:2010
EN ISO 4499-2:2010 (E)
Contents Page
Foreword .3

2

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SIST EN ISO 4499-2:2010
EN ISO 4499-2:2010 (E)
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 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 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 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 24499:1993.
ISO 4499-2, together with ISO 4499-1, cancels and replaces ISO 4499:1978, which has been technically
revised. 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 grain 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, 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.

3

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SIST EN ISO 4499-2:2010

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SIST EN ISO 4499-2:2010

INTERNATIONAL ISO
STANDARD 4499-2
First edition
2008-09-15


Hardmetals — Metallographic
determination of microstructure —
Part 2:
Measurement of WC grain size
Métaux-durs — Détermination métallographique de la microstructure —
Partie 2: Mesurage de la taille des grains de WC




Reference number
ISO 4499-2:2008(E)
©
ISO 2008

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
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ii © ISO 2008 – All rights reserved

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
Contents Page
Foreword. iv
1 Scope .1
2 Normative references .2
3 Terms, definitions, abbreviations, symbols and units.2
4 General information.4
5 Apparatus .5
6 Calibration .6
7 Grain-size measurement by the linear-intercept method .6
8 Reporting .9
Annex A (informative) Measurement case study .11
Annex B (informative) Report proforma.15
Bibliography .17

© ISO 2008 – All rights reserved iii

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
Foreword
ISO (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 technical 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 of electrotechnical standardization.
International Standards are 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
International Standard requires approval by at least 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 4499-2 was prepared by Technical Committee ISO/TC 119, Powder metallurgy, Subcommittee SC 4,
Sampling and testing methods for hardmetals.
ISO 4499-2, together with ISO 4499-1, cancels and replaces ISO 4499:1978, which has been technically
revised. 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 grain size

iv © ISO 2008 – All rights reserved

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SIST EN ISO 4499-2:2010
INTERNATIONAL STANDARD ISO 4499-2:2008(E)

Hardmetals — Metallographic determination of
microstructure —
Part 2:
Measurement of WC grain size
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) containing 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 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 ISO 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 is
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.
© ISO 2008 – All rights reserved 1

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
2 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 3326, 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: Preparation 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 determination 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 Fine Microfine
Coarse Very fine Micrograin
Coarse/Medium Ultra fine Nanophase
Medium Extra 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 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 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 µm as Nano/Ultrafine 0,21 µm as Ultrafine/Nano
0,75 µm as Submicron/Fine 0,85 µm as Fine/Submicron
1,29 µm as Fine/Medium 1,31 µm as Medium/Fine
2,4 µm as Medium/Coarse 2,6 µm as Coarse/Medium
2 © ISO 2008 – All rights reserved

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
3.2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.2.1
nano
with WC grain size < 0,2 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.2
ultrafine
with WC grain size 0,2 µm to 0,5 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.3
submicron
with WC grain size 0,5 µm to 0,8 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.4
fine
with WC grain size 0,8 µm to 1,3 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.5
medium
with WC grain size 1,3 µm to 2,5 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.6
coarse
with WC grain size 2,5 µm to 6,0 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.7
extra coarse
with WC grain size > 6,0 µm
NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.3 Symbols, abbreviations and units
For the purposes of this document, the following symbols, abbreviations and units apply.
2
A is the area, in square millimetres (mm)
is the arithmetic mean linear intercept of WC grains, in micrometres (µm)
d

wc
ECD is the equivalent circle diameter, in millimetres (mm)
L is the line length, in millimetres (mm)
© ISO 2008 – All rights reserved 3

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
LI is the arithmetic mean-linear-intercept distance, in micrometres (µm)
l is the measured length of individual intercepts, in micrometres (µm)
i
l is the sum of the measured length of each individual intercept
∑ i
N is the number of grain boundaries traversed
n is the number of WC grains intercepted
m is the magnification
m is the maximum magnification
max
m is the minimum magnification
min
s is the measured size, in millimetres (mm)
m
is the actual size, in millimetres (mm)
s
a
4 General information
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 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 improving 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), 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-section 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 2D 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 parameter
counted.
4 © ISO 2008 – All rights reserved

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SIST EN ISO 4499-2:2010
ISO 4499-2:2008(E)
The value most used to date has been a length parameter. This can be obtained in several ways, for example,
[12]
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;
1)
⎯ by the equivalent circle diameter ; 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, 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 linear-intercept method.
5 Apparatus
[10]
Grain-size measurements are obtained from images of the microstructure. ISO 4499-1, ASTM B657 and
[11]
ASTM B665 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 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 semiautomatically
using image analysis. Automatic image analysis can be used in some circumstances when the images are
fairly coarse and good contrast can be obtained, but for many materials, especially those with very fine grain
sizes, good images are difficult to acquire and are generally not amenable to automatic analysis.
For the ultrafine and nano grades, good images are particularly difficult to acquire using conventional
scanning electron microscopes with tungsten-filament electron sources. For these materials, it is
recommended that a field emission SEM (FESEM) be used. These systems give significantly higher resolution
images, sufficient to measure materials with mean intercept sizes of about 0,1 µm to 0,2 µm. For materials
with ever smaller grain sizes, it may be necessary to use transmission electron microscopy (TEM). However,
the problems of sampling and specimen preparation are particularly severe (see [7] in the Bibliography).
Careful specimen preparation for good images is vital for these materials, and often a combination of etching
methods is helpful (see ISO 4499-1).

1) It is possible, for equiaxed grains, to convert an equivalent circle diameter (ECD) grain size to a linear intercept (LI)
value using Equation [
...

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 2: Messung der WC Korngröße (ISO 4499-2:2008)Métaux-durs - Détermination métallographique de la microstructure - Partie 2: Mesurage de la taille des grains de WC (ISO 4499-2:2008)Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2008)77.160Metalurgija prahovPowder metallurgy77.040.99Druge metode za preskušanje kovinOther methods of testing of metalsICS:Ta slovenski standard je istoveten z:FprEN ISO 4499-2kSIST FprEN ISO 4499-2:2010en,fr,de01-januar-2010kSIST FprEN ISO 4499-2:2010SLOVENSKI
STANDARD



kSIST FprEN ISO 4499-2:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN ISO 4499-2
October 2009 ICS 77.040.99; 77.160 Will supersede EN 24499:1993English Version
Hardmetals - Metallographic determination of microstructure - Part 2: Measurement of WC grain size (ISO 4499-2:2008)
Métaux-durs - Détermination métallographique de la microstructure - Partie 2: Mesurage de la taille des grains de WC (ISO 4499-2:2008)
Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 2: Messung der WC Korngröße (ISO 4499-2:2008) This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical Committee CEN/SS M11.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 Management Centre has the same status as the official versions.
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Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and shall not be referred to as a European Standard.
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FprEN ISO 4499-2:2009 (E) 2 Contents Page Foreword .3 kSIST FprEN ISO 4499-2:2010



FprEN ISO 4499-2:2009 (E) 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 FprEN ISO 4499-2:2009. This document is currently submitted to the Unique Acceptance Procedure. This document will supersede EN 24499:1993. ISO 4499-2, together with ISO 4499-1, cancels and replaces ISO 4499:1978, which has been technically revised. 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 grain size Endorsement notice The text of ISO 4499-2:2008 has been approved by CEN as a FprEN ISO 4499-2:2009 without any modification.
kSIST FprEN ISO 4499-2:2010



kSIST FprEN ISO 4499-2:2010



Reference numberISO 4499-2:2008(E)© ISO 2008
INTERNATIONAL STANDARD ISO4499-2First edition2008-09-15Hardmetals — Metallographic determination of microstructure — Part 2: Measurement of WC grain size Métaux-durs — Détermination métallographique de la microstructure —Partie 2: Mesurage de la taille des grains de WC
kSIST FprEN ISO 4499-2:2010



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kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) © ISO 2008 – All rights reserved iiiContents Page Foreword.iv 1 Scope.1 2 Normative references.2 3 Terms, definitions, abbreviations, symbols and units.2 4 General information.4 5 Apparatus.5 6 Calibration.6 7 Grain-size measurement by the linear-intercept method.6 8 Reporting.9 Annex A (informative)
Measurement case study.11 Annex B (informative)
Report proforma.15 Bibliography.17
kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) iv © ISO 2008 – All rights reserved Foreword ISO (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 technical 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 of electrotechnical standardization. International Standards are 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 International Standard requires approval by at least 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 4499-2 was prepared by Technical Committee ISO/TC 119, Powder metallurgy, Subcommittee SC 4, Sampling and testing methods for hardmetals. ISO 4499-2, together with ISO 4499-1, cancels and replaces ISO 4499:1978, which has been technically revised. 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 grain size
kSIST FprEN ISO 4499-2:2010



INTERNATIONAL STANDARD ISO 4499-2:2008(E) © ISO 2008 – All rights reserved 1Hardmetals — Metallographic determination of microstructure — Part 2: Measurement of WC grain size 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) containing 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 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 ISO 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 is 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. kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) 2 © ISO 2008 – All rights reserved 2 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 3326, 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: Preparation 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 determination 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 Fine Microfine Coarse Very fine Micrograin Coarse/Medium Ultra fine Nanophase Medium Extra 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 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 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 µm as Nano/Ultrafine 0,21 µm as Ultrafine/Nano 0,75 µm as Submicron/Fine 0,85 µm as Fine/Submicron 1,29 µm as Fine/Medium 1,31 µm as Medium/Fine 2,4 µm as Medium/Coarse 2,6 µm as Coarse/Medium kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) © ISO 2008 – All rights reserved 33.2 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.2.1 nano with WC grain size < 0,2 µm NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.2 ultrafine with WC grain size 0,2 µm to 0,5 µm NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.3 submicron with WC grain size 0,5 µm to 0,8 µm NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.4 fine with WC grain size 0,8 µm to 1,3 µm NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.5 medium with WC grain size 1,3 µm to 2,5 µm NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.6 coarse with WC grain size 2,5 µm to 6,0 µm NOTE Measured by the mean-linear-intercept method described in this part of ISO 4499.
3.2.7 extra coarse with WC grain size > 6,0 µm NOTE Measured by the mean-linear-intercept method described in this part 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 (µm) ECD is the equivalent circle diameter, in millimetres (mm)
L is the line length, in millimetres (mm) kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) 4 © ISO 2008 – All rights reserved LI is the arithmetic mean-linear-intercept distance, in micrometres (µm) il is the measured length of individual intercepts, in micrometres (µm) il∑ is the sum of the measured length of each 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 information 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 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 improving 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), 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-section 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 2D 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 parameter counted. kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) © ISO 2008 – All rights reserved 5The 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 E112[12]: ⎯ by linear intercept, called the Heyn method, from a straight line drawn 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, 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 linear-intercept method. 5 Apparatus Grain-size measurements are obtained from images of the microstructure. ISO 4499-1, ASTM B657 [10] and 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 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 semiautomatically using image analysis. Automatic image analysis can be used in some circumstances when the images are fairly coarse and good contrast can be obtained, but for many materials, especially those with very fine grain sizes, good images are difficult to acquire and are generally not amenable to automatic analysis. For the ultrafine and nano grades, good images are particularly difficult to acquire using conventional scanning electron microscopes with tungsten-filament electron sources. For these materials, it is recommended that a field emission SEM (FESEM) be used. These systems give significantly higher resolution images, sufficient to measure materials with mean intercept sizes of about 0,1 µm to 0,2 µm. For materials with ever smaller grain sizes, it may be necessary to use transmission electron microscopy (TEM). However, the problems of sampling and specimen preparation are particularly severe (see [7] in the Bibliography). Careful specimen preparation for good images is vital for these materials, and often a combination of etching methods is helpful (see ISO 4499-1).
1) It is possible, for equiaxed grains, to convert an equivalent circle diameter (ECD) grain size to a linear intercept (LI) value using Equation [1]. LI/4ECDA==π (1) Thus ECD = 1,13 LI This expression is discussed in References [1] and [5] in the Bibliography. kSIST FprEN ISO 4499-2:2010



ISO 4499-2:2008(E) 6 © ISO 2008 – All rights reserved 6 Calibration To give reliable quantitative measurements, images shall be calibrated against a stage micrometer or scale traceable to a National Referenc
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