SIST EN ISO 4499-3:2016
(Main)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)
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
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 4499-3:2016
01-maj-2016
7UGLQH0HWDORJUDIVNRGRORþHYDQMHPLNURVWUXNWXUHGHO 0HUMHQMH
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
2
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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.
3
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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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
---------------------- Page: 8 ----------------------
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
2
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)
i
l
sum of the measured length of each individual intercept
∑
i
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)
x
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
...
SLOVENSKI STANDARD
oSIST prEN ISO 4499-3:2014
01-maj-2014
7UGLQH0HWDORJUDIVNRGRORþHYDQMHPLNURVWUXNWXUHGHO 0HUMHQMH
PLNURVWUXNWXUQLK]QDþLOQRVWLYWUGLQDKQDRVQRYL7L &1 LQ:&NXELþQHJDNDUELGD
,62',6
Hardmetals - Metallographic determination of microstructure - Part 3: Measurement of
microstructural features in Ti (C, N) and WC/Cubic Carbide Based Hardmetals (ISO/DIS
4499-3:2014)
Hartmetalle - Metallographische Bestimmung der Mikrostruktur - Teil 3: Messung von
mikrostrukturellen Merkmalen in Hartmetallen auf Basis von Ti (C, N) und WC/kubischem
Carbid (ISO/DIS 4499-3:2014)
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/DIS 4499-3:2014)
Ta slovenski standard je istoveten z: prEN ISO 4499-3
ICS:
77.040.99 Druge metode za Other methods of testing of
preskušanje kovin metals
77.160 Metalurgija prahov Powder metallurgy
oSIST prEN ISO 4499-3:2014 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 4499-3:2014
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oSIST prEN ISO 4499-3:2014
DRAFT INTERNATIONAL STANDARD
ISO/DIS 4499-3
ISO/TC 119/SC 4 Secretariat: DIN
Voting begins on: Voting terminates on:
2014-03-13 2014-08-13
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
ICS: 77.040.99;77.160
ISO/CEN PARALLEL PROCESSING
This draft has been developed within the International Organization for
Standardization (ISO), and processed under the ISO lead mode of collaboration
as defined in the Vienna Agreement.
This draft is hereby submitted to the ISO member bodies and to the CEN member
bodies for a parallel five month enquiry.
Should this draft be accepted, a final draft, established on the basis of comments
received, will be submitted to a parallel two-month approval vote in ISO and
THIS DOCUMENT IS A DRAFT CIRCULATED
formal vote in CEN.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
To expedite distribution, this document is circulated as received from the
IN ADDITION TO THEIR EVALUATION AS
committee secretariat. ISO Central Secretariat work of editing and text
BEING ACCEPTABLE FOR INDUSTRIAL,
composition will be undertaken at publication stage.
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 4499-3:2014(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2014
---------------------- Page: 3 ----------------------
oSIST prEN ISO 4499-3:2014
ISO/DIS 4499-3:2014(E)
Copyright notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as
permitted under the applicable laws of the user’s country, neither this ISO draft nor any extract
from it may be reproduced, stored in a retrieval system or transmitted in any form or by any means,
electronic, photocopying, recording or otherwise, without prior written permission being secured.
Requests for permission to reproduce should be addressed to either ISO at the address below or ISO’s
member body in the country of the requester.
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Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
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Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
ii © ISO 2014 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 4499-3:2014
ISO/DIS 4499-3
Contents Page
Foreword . iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and units . 3
5 Principle. 3
6 Apparatus . 4
7 Calibration . 4
8 Preparation of test samples . 5
8.1 Metallographic preparation . 5
8.2 Ti(C, N) Based Hardmetals – Cermets . 5
8.3 WC/Cubic Carbide Based Hardmetals . 9
9 Procedure for Characterisation of Structures . 18
9.1 Sampling of Images of Structure . 18
9.1.1 General . 18
9.1.2 Representative selection . 18
9.1.3 Determination of homogeneity of hard phase sizes . 18
9.1.4 Inhomogeneous materials . 18
9.2 Phase Size Measurement. 18
9.2.1 Phase measurement by intercepts . 19
10 Uncertainty of Measurement . 21
11 Test report . 22
Bibliography . 23
© ISO 2013 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 4499-3:2014
ISO/DIS 4499-3
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 4499-3 was prepared by Technical Committee 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
Part 5: Characterisation and measurement of miscellaneous microstructural features
iv © ISO 2013 – All rights reserved
---------------------- Page: 6 ----------------------
oSIST prEN ISO 4499-3:2014
ISO/DIS 4499-3
Introduction
This part of ISO 4499 essentially covers the following topics:
materials types and phases to be measured including:
a) Ti(C, N) cermets
b) 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 2013 – All rights reserved v
---------------------- Page: 7 ----------------------
oSIST prEN ISO 4499-3:2014
---------------------- Page: 8 ----------------------
oSIST prEN ISO 4499-3:2014
DRAFT INTERNATIONAL STANDARD ISO/DIS 4499-3
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 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 4499-1, Hardmetals — Metallographic determination of microstructure — Part 1: Photomicrographs and
description
ISO 4499-2, Hardmetals — Metallographic determination of microstructure — Part 2: Measurement of WC
grain size
ASTM B 657, Guide for Metallographic Identification of Microstructure in Cemented Carbides
ASTM B 665, Standard Guide for Metallographic Sample Preparation of Cemented Tungsten Carbides
ASTM E 112, Standard Test Methods for Determining Average Grain Size
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
nano
with carbonitride or, respectively, cubic carbide phase size < 0,2 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
3.2
ultrafine
with carbonitride or, respectively, cubic carbide phase size 0,2 µm to 0,5 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
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3.3
submicron
with carbonitride or, respectively, cubic carbide phase size 0,5 µm to 0,8 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
3.4
fine
with carbonitride or, respectively, cubic carbide phase size 0,8 µm to 1,3 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
3.5
medium
with carbonitride or, respectively, cubic carbide phase size 1,3 µm to 2,5 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
3.6
coarse
with carbonitride or, respectively, cubic carbide phase size 2,5 µm to 6,0 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
3.7
extra coarse
with carbonitride or, respectively, cubic carbide phase size > 6,0 µm
Note 1 to entry: Measured by the mean-linear-intercept method described in ISO 4499-2.
3.8
Ti(C, N) cermets
a TiCN-based cermet contains 3-30 weight % of a binder phase mainly composed of Co and/or Ni, but also
may include Mo; the balance being substantially a hard phase and a few minor impurities
Note 1 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 2 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.
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4 Symbols and units
For the purposes of this document, the following symbols, abbreviations and units apply.
2
A is the area, in square millimetres (mm)
ECD is the equivalent circle diameter, in micrometres (µm), of a specified phase
L is the total line length, in millimetres (mm), in a specified phase
l is the measured length of individual intercepts, in micrometres (µm), in a specified phase
i
l is the sum of the measured length of each individual intercept
i
∑
is the arithmetic mean linear intercept in phase x, in micrometres (µm)
l
x
N is the number of grain boundaries traversed in or between specified phases
n is the number of WC, carbonitride or cubic carbide grains intercepted
m is the magnification
m is the maximum magnification
max
m is the 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, [1-2]). 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 based on TiC or Ti(C,N) [3-5]. 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 an Appendix
Case Study in this part of ISO 4499.
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.
There are three ways by which the mean size by number of the various phases can be defined:
by length (of a line across a 2D section of a phase);
by area (of 2D sections of phase regions);
by volume (of individual phase regions).
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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.
The values for phase size most used to date have been based on a length parameter. This can be obtained in
several ways, for example, by parallel lines or circles as described in ASTM E112:
by linear intercept, called the Heyn method, from a straight line drawn across the structure;
by equivalent circle diameter (see ISO 4499-2), this is obtained by measuring hard phase grain areas and
then taking the diameter of a circle of equivalent area.
6 Apparatus
6.1 Metallographic optical microscope, or other suitable equipment permitting observations and
measurements on a screen up to the required magnification.
6.2 Scanning electron microscope, permitting observations and measurements of features too small to be
resolved with an optical microscope.
6.3 Equipment for preparation of test-piece sections.
Phase size measurements are obtained from images of the microstructure. ISO 4499-1, ASTM B 657 and
ASTM B 665 should be consulted for best practice in the preparation of surfaces for imaging.
Structural images are usually generated by either optical microscopy or Scanning Electron Microscopy (SEM).
For accurate measurements it is better to use scanning electron microscopic images. Even in coar
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