Hardmetals - Metallographic determination of microstructure - Part 3: Measurement of microstructural features in Ti (C, N) and WC/cubic carbide based hardmetals (ISO 4499-3:2016)

This 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 called
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.

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)

Métaux-durs - Détermination métallographique de la microstructure - Partie 3: Mesure des caractéristiques des microstructures des métaux-durs à base de carbures Ti (C, N) et WC/cubiques (ISO 4499-3:2016)

L'ISO 4499-3:2016 donne des lignes directrices relatives à la mesure des caractéristiques des microstructures des métaux-durs à base de carbures Ti(C,N) et de métaux-durs WC/Co contenant des carbures cubiques supplémentaires selon des techniques métallographiques utilisant uniquement un microscope optique ou électronique. Elle est destinée aux métaux-durs frittés (également appelés carbures cémentés ou cermets) contenant principalement des carbures et nitrures inorganiques sous la forme d'une phase dure. Elle est également destinée au mesurage de la taille des phases et de la distribution au moyen de la technique d'interception linéaire.

Trdine - Metalografsko določevanje mikrostrukture - 3. del: Merjenje mikrostrukturnih značilnosti v trdinah na osnovi Ti (C, N) in WC/kubičnega karbida (ISO 4499-3:2016)

Ta del standarda ISO 4499 podaja navodila za merjenje mikrostrukturnih značilnosti v trdinah na osnovi Ti (C, N) in WC/kubičnega karbida, ki vsebujejo dodatne kubične karbide, na podlagi metalografskih tehnik, ki uporabljajo le optično mikroskopijo ali mikroskopijo elektronov. Uporablja se za sintrane trdine (imenovane tudi cementirani karbidi ali cermeti), ki v trdi fazi vsebujejo pretežno anorganske karbide in nitride. Namenjen je tudi merjenju velikosti in distribucije faze s tehniko linearnega prestrezanja.

General Information

Status
Published
Public Enquiry End Date
29-Jun-2014
Publication Date
10-Apr-2016
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
24-Mar-2016
Due Date
29-May-2016
Completion Date
11-Apr-2016

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SLOVENSKI STANDARD
SIST EN ISO 4499-3:2016
01-maj-2016
7UGLQH0HWDORJUDIVNRGRORþHYDQMHPLNURVWUXNWXUHGHO0HUMHQMH

PLNURVWUXNWXUQLK]QDþLOQRVWLYWUGLQDKQDRVQRYL7L &1 LQ:&NXELþQHJDNDUELGD

,62

Hardmetals - Metallographic determination of microstructure - Part 3: Measurement of

microstructural features in Ti (C, N) and WC/cubic carbide based hardmetals (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)

Métaux-durs - Détermination métallographique de la microstructure - Partie 3: Mesure

des caractéristiques des microstructures des métaux-durs à base de carbures Ti (C, N)

et WC/cubiques (ISO 4499-3:2016)
Ta slovenski standard je istoveten z: EN ISO 4499-3:2016
ICS:
77.040.99 Druge metode za Other methods of testing of
preskušanje kovin metals
77.160 Metalurgija prahov Powder metallurgy
SIST EN ISO 4499-3:2016 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 4499-3:2016
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SIST EN ISO 4499-3:2016
EN ISO 4499-3
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2016
EUROPÄISCHE NORM
ICS 77.040.99; 77.160
English Version
Hardmetals - Metallographic determination of
microstructure - Part 3: Measurement of microstructural
features in Ti (C, N) and WC/cubic carbide based
hardmetals (ISO 4499-3:2016)

Métaux-durs - Détermination métallographique de la Hartmetalle - Metallographische Bestimmung der

microstructure - Partie 3: Mesure des caractéristiques Mikrostruktur - Teil 3: Messung von

des microstructures des métaux-durs à base de mikrostrukturellen Merkmalen in Hartmetallen auf

carbures Ti (C, N) et WC/cubiques (ISO 4499-3:2016) Basis von Ti (C, N) und WC/kubischem Carbid (ISO

4499-3:2016)
This European Standard was approved by CEN on 4 February 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 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 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, 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 and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR 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 Ref. No. EN ISO 4499-3:2016 E

worldwide for CEN national Members.
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SIST EN ISO 4499-3:2016
EN ISO 4499-3:2016 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 4499-3:2016
EN ISO 4499-3:2016 (E)
European foreword

This document (EN ISO 4499-3:2016) has been prepared by Technical 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 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 not be held responsible for identifying any or all such patent

rights.

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, 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 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.
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SIST EN ISO 4499-3:2016
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SIST EN ISO 4499-3:2016
INTERNATIONAL ISO
STANDARD 4499-3
First edition
2016-02-15
Hardmetals — Metallographic
determination of microstructure —
Part 3:
Measurement of microstructural
features in Ti (C, N) and WC/cubic
carbide based hardmetals
Métaux-durs — Détermination métallographique de la
microstructure —
Partie 3: Mesure des caractéristiques des microstructures des métaux-
durs à base de carbures Ti (C, N) et WC/cubiques
Reference number
ISO 4499-3:2016(E)
ISO 2016
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SIST EN ISO 4499-3:2016
ISO 4499-3:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior

written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of

the requester.
ISO copyright office
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copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
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SIST EN ISO 4499-3:2016
ISO 4499-3:2016(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Symbols and units ............................................................................................................................................................................................... 2

5 Principle ........................................................................................................................................................................................................................ 3

6 Apparatus ..................................................................................................................................................................................................................... 3

7 Calibration .................................................................................................................................................................................................................. 4

8 Preparation of test samples ...................................................................................................................................................................... 4

8.1 Metallographic preparation ......................................................................................................................................................... 4

8.2 Ti(C, N) based hardmetals – cermets................................................................................................................................... 4

8.3 WC/Cubic carbide based hardmetals .................................................................................................................................. 8

9 Procedure for characterisation of structures......................................................................................................................20

9.1 Sampling of images of structure ...........................................................................................................................................20

9.1.1 General...................................................................................................................................................................................20

9.1.2 Representative selection ........................................................................................................................................20

9.1.3 Determination of homogeneity of hard phase sizes .......................................................................20

9.1.4 Inhomogeneous materials ....................................................................................................................................21

9.2 Phase size measurement .............................................................................................................................................................21

9.2.1 General...................................................................................................................................................................................21

9.2.2 Phase measurement by intercepts ................................................................................................................21

10 Uncertainty of measurement ................................................................................................................................................................23

11 Test report ................................................................................................................................................................................................................23

Bibliography .............................................................................................................................................................................................................................25

© ISO 2016 – All rights reserved iii
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SIST EN ISO 4499-3:2016
ISO 4499-3:2016(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.

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 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 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 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 not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s 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 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

— Part 4: Characterisation of porosity, carbon defects and eta-phase content
iv © ISO 2016 – All rights reserved
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SIST EN ISO 4499-3:2016
ISO 4499-3:2016(E)
Introduction
This part of ISO 4499 essentially covers the following topics:
— materials types and phases to be measured including the following:
— Ti(C, N) cermets;
— 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 average values;
— reporting to comply with modern quality requirements.
© ISO 2016 – All rights reserved v
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SIST EN ISO 4499-3:2016
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SIST EN ISO 4499-3:2016
INTERNATIONAL STANDARD ISO 4499-3:2016(E)
Hardmetals — Metallographic determination of
microstructure —
Part 3:
Measurement of microstructural features in Ti (C, N) and
WC/cubic carbide based hardmetals
1 Scope

This 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 called

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 references

The 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 latest edition of the referenced document (including any amendments) applies.

ISO 4499–1:2008, Hardmetals — Metallographic determination of microstructure — Part 1:

Photomicrographs and description

ISO 4499–2:2008, Hardmetals — Metallographic determination of microstructure — Part 2: Measurement

of WC grain size
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
nano
with carbonitride or cubic carbide phase size <0,2 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

3.2
ultrafine
with carbonitride or cubic carbide phase size 0,2 µm to 0,5 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

3.3
submicron
with carbonitride or cubic carbide phase size 0,5 µm to 0,8 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

© ISO 2016 – All rights reserved 1
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SIST EN ISO 4499-3:2016
ISO 4499-3:2016(E)
3.4
fine
with carbonitride or cubic carbide phase size 0,8 µm to 1,3 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

3.5
medium
with carbonitride or cubic carbide phase size 1,3 µm to 2,5 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

3.6
coarse
with carbonitride or cubic carbide phase size 2,5 µm to 6,0 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

3.7
extra coarse
with carbonitride or cubic carbide phase size >6,0 µm, respectively

Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.

3.8
Ti(C, N) cermets

TiCN-based cermet contains 3 to 30 weight % of a binder phase mainly composed of Co and/or Ni, but

may also include Mo

Note 1 to entry: The balance being substantially a hard phase 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 structure.

3.9
WC/Cubic carbide hardmetals

hexagonal 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 solution

Note 1 to entry: These materials typically contain hard phases that may have grains with a core/rim structure.

Note 2 to entry: See Table 1.
3.10
phase region
single constituent of the hardmetal like WC, cubic carbide or binder
4 Symbols and units
A area, in square millimetres (mm )
ECD Equivalent Circle Diameter of a specified phase, in micrometres (μm)
L total line length in a specified phase, in millimetres (mm)

l measured length of individual intercepts in a specified phase, in micrometres (µm)

sum of the measured length of each individual intercept
2 © ISO 2016 – All rights reserved
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SIST EN ISO 4499-3:2016
ISO 4499-3:2016(E)
l arithmetic mean linear intercept in phase x, in micrometres (µm)
N number of grain boundaries traversed in or between specified phases
n number of WC, carbonitride or cubic carbide grains intercepted
m magnification
m maximum magnification
max
m minimum magnification
min
5 Principle

This part of ISO 4499 addresses the issue of good practice for the measurement of a mean value for 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 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

types of hardmetal considered are those that contain cubic carbides as well as WC and those that are

[3][4][5]

based on TiC or Ti(C,N). A 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.

These materials typically contain hard phases that have grains with a core/rim structure. Guidelines to

measure these internal details are included in ISO 4499–2:2008, 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 quantitative 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
...

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