SIST EN ISO 13383-1:2016
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural characterization - Part 1: Determination of grain size and size distribution (ISO 13383-1:2012)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural characterization - Part 1: Determination of grain size and size distribution (ISO 13383-1:2012)
This part of ISO 13383 describes manual methods of making measurements for the determination of grain size of fine ceramics (advanced ceramics, advanced technical ceramics) using photomicrographs of polished and etched test pieces. The methods described in this part do not yield the true mean grain diameter, but a somewhat smaller parameter depending on the method applied to analyse a two-dimensional section. The relationship to true grain dimensions depends on the grain shape and the degree of microstructural anisotropy. This part contains two principal methods, A and B.
Method A is the mean linear intercept technique. Method A1 applies to single-phase ceramics, and to ceramics with a principal crystalline phase and a glassy grain-boundary phase of less than about 5 % by volume for which intercept counting suffices. Method A2 applies to ceramics with more than about 5 % by volume of pores or secondary phases, or ceramics with more than one major crystalline phase where individual intercept lengths are measured, which can optionally be used to create a size distribution. This latter method allows the pores or phases to be distinguished and the mean linear intercept size for each to be calculated separately.
Method B is the mean equivalent circle diameter method, which applies to any type of ceramic with or without a secondary phase. This method may also be employed for determining grain aspect ratio and a size distribution.
Some users of this part of ISO 13383 may wish to apply automatic or semiautomatic image analysis to micrographs or directly captured microstructural images. This is permitted by this part provided that the technique employed simulates the manual methods (see Clause 4 and 8.4).
Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 1: Bestimmung der Korngröße und der Korngrößenverteilung (ISO 13383-1:2012)
Dieser Teil von ISO 13383 beschreibt manuelle Messverfahren zur Bestimmung der Korngröße von Hoch¬leistungskeramik unter Verwendung von mikrophotographischen Aufnahmen polierter und geätzter Proben. Die in diesem Teil beschriebenen Verfahren ergeben nicht den wahren mittleren Korndurchmesser, sondern einen etwas kleineren Wert, je nach dem zur Analyse eines zweidimensionalen Probenquerschnitts ange¬wandten Verfahren. Der Zusammenhang mit den wahren Kornmaßen hängt von der Kornform und vom Anisotropiegrad des Mikrogefüges ab. Dieser Teil enthält zwei Verfahren, Verfahren A und Verfahren B.
Das Verfahren A ist das Verfahren zur Bestimmung der mittleren Schnittlinienlänge (Linienschnitt¬ver-fahren). Das Verfahren A1 gilt für einphasige Keramikwerkstoffe mit einer kristallinen Hauptphase und einer glasigen Korngrenzenphase mit einem Volumenanteil von höchstens etwa 5 %, bei denen das Auszählen der Schnittpunkte genügt. Das Verfahren A2 gilt für Keramikwerkstoffe mit einem Volumenanteil von über etwa 5 % Poren oder Sekundärphasen oder für Keramikwerkstoffe mit mehr als einer kristallinen Hauptphase, bei denen einzelne Schnittlinienlängen gemessen werden, die wahlweise auch zur Bestimmung der Korn¬größenverteilung verwendet werden können. Bei letzterem Verfahren können Poren oder Phasen unter¬schieden werden und für jede kann die mittlere, aus der Schnittlinienlänge bestimmte Korngröße separat bestimmt werden.
ANMERKUNG Ein Verfahren zur Bestimmung des/der Volumenanteils/Volumenanteile der Sekundärphase(n) kann ISO 13383 2 entnommen werden; es bietet in Grenzfällen Entscheidungsmöglichkeiten dafür an, ob Verfahren A1 oder Verfahren A2 angewendet werden sollte.
Das Verfahren B ist das Verfahren zur Bestimmung des mittleren Kreisäquivalentdurchmessers, das bei allen Keramikwerkstoffen mit oder ohne Sekundärphase anwendbar ist. Dieses Verfahren darf auch zur Bestim¬mung des Seitenverhältnisses der Körner und zur Bestimmung der Korngrößenverteilung ange¬wendet werden.
Es kann sein, dass einige Anwender dieses Teils von ISO 13383 eine automatische oder halbautomatische Bildanalyse auf die Mikrogefügeaufnahmen oder auf direkt angezeigte Gefügebilder anwenden möchten. Die Anwendung dieser Analysenverfahren ist nach diesem Teil unter der Voraussetzung zulässig, dass eine den manuellen Verfahren entsprechende Technik eingesetzt wird (siehe Abschnitt 4 und 8.4).
Céramiques techniques - Caractérisation microstructurale - Partie 1: Détermination de la grosseur du grain et de la distribution granulométrique (ISO 13383-1:2012)
L'ISO 13383-1:2012 décrit des méthodes manuelles de mesurage permettant de déterminer la taille de grain de céramiques techniques en utilisant des micrographies d'éprouvettes polies et soumises à une attaque. Les méthodes décrites dans l'ISO 13383-1:2012 ne donnent pas le diamètre moyen vrai du grain, mais un paramètre relativement plus faible selon la méthode appliquée pour analyser une section bidimensionnelle. La relation par rapport aux dimensions vraies du grain dépend de la forme du grain et du degré d'anisotropie de la microstructure. L'ISO 13383-1:2012 contient deux méthodes principales, A et B.
La méthode A est la technique de la moyenne des interceptions linéaires. La méthode A1 s'applique aux céramiques monophasées et aux céramiques ayant une phase cristalline principale et une phase vitreuse au niveau des joints de grains de moins de 5 % environ en volume pour laquelle un comptage des interceptions suffit. La méthode A2 s'applique aux céramiques ayant plus de 5 % environ en volume de pores ou de phases secondaires ou aux céramiques ayant plus d'une phase cristalline principale dans lesquelles les longueurs d'interception individuelles sont mesurées, et peuvent éventuellement être utilisées pour établir une distribution granulométrique. Cette dernière méthode permet de faire la distinction entre les pores et les phases et de calculer séparément la taille moyenne des interceptions de chacun.
La méthode B est la méthode du diamètre du cercle moyen équivalent qui s'applique à tout type de céramique avec ou sans phase secondaire. Cette méthode peut également être employée pour la détermination du rapport de forme des grains et de la distribution granulométrique.
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Značilnosti mikrostrukture - 1. del: Določanje velikosti zrn in porazdelitve velikosti (ISO 13383-1:2012)
Ta del standarda ISO 13383 opisuje ročne metode merjenja za določanje velikosti zrn fine keramike (sodobne keramike, sodobne tehnične keramike) s fotomikrografi poliranih in jedkanih testnih kosov. Z metodo, opisano v tem delu, se ne ugotovi pravega povprečnega premera zrn, ampak nekoliko manjši premer, odvisno od uporabljene metode za analizo dvorazsežnega preseka. Razmerje s pravimi merami zrn je odvisno od oblike zrn in stopnje mikrostrukturne anizotropije. Ta del vsebuje dve osnovni metodi, A in B. Metoda A je tehnika povprečnega linearnega preseka. Metoda A1 se uporablja za enofazno keramiko ter keramiko z osnovno kristalinično fazo in fazo steklaste meje zrn, ki zajema manj kot 5 % prostornine, za katero zadošča štetje preseka. Metoda A2 se uporablja za keramiko z več kot okoli 5 % prostornine por ali sekundarnih faz ali keramiko z več kot eno glavno kristalinično fazo, kjer se meri posamezne dolžine presekov, kar je mogoče izbirno uporabiti za ugotavljanje porazdelitve velikosti. Druga metoda omogoča razlikovanje por ali faz in ločen izračun povprečne linearne velikosti preseka za vsako od njih. Metoda B je metoda povprečnega enakovrednega premera kroga, ki se uporablja za vse vrste keramike ne glede na to, ali imajo sekundarno fazo ali ne. To metodo je mogoče uporabiti tudi za določanje razmerja med višino in širino zrn ter porazdelitve velikosti. Nekateri uporabniki tega dela standarda ISO 13383 bodo morda želeli za mikrografe ali neposredno zajete mikrostrukturne slike uporabiti samodejno ali polsamodejno analizo slik. Ta del to dovoljuje pod pogojem, da uporabljena tehnika simulira ročne metode (glej točki 4 in 8.4).
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 13383-1:2016
01-junij-2016
1DGRPHãþD
SIST EN 623-3:2002
)LQDNHUDPLND VRGREQDNHUDPLNDVRGREQDWHKQLþQDNHUDPLND =QDþLOQRVWL
PLNURVWUXNWXUHGHO 'RORþDQMHYHOLNRVWL]UQLQSRUD]GHOLWYHYHOLNRVWL ,62
Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural
characterization - Part 1: Determination of grain size and size distribution (ISO 13383-
1:2012)
Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 1: Bestimmung der
Korngröße und der Korngrößenverteilung (ISO 13383-1:2012)
Céramiques techniques - Caractérisation microstructurale - Partie 1: Détermination de la
grosseur du grain et de la distribution granulométrique (ISO 13383-1:2012)
Ta slovenski standard je istoveten z: EN ISO 13383-1:2016
ICS:
81.060.30 Sodobna keramika Advanced ceramics
SIST EN ISO 13383-1:2016 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 13383-1:2016
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SIST EN ISO 13383-1:2016
EN ISO 13383-1
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2016
EUROPÄISCHE NORM
ICS 81.060.30 Supersedes EN 623-3:2001
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Microstructural characterization - Part 1:
Determination of grain size and size distribution (ISO
13383-1:2012)
Céramiques techniques - Caractérisation Hochleistungskeramik - Mikrostrukturelle
microstructurale - Partie 1: Détermination de la taille Charakterisierung - Teil 1: Bestimmung der Korngröße
et de la distribution des grains (ISO 13383-1:2012) und der Korngrößenverteilung (ISO 13383-1:2012)
This European Standard was approved by CEN on 18 March 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 13383-1:2016 E
worldwide for CEN national Members.
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SIST EN ISO 13383-1:2016
EN ISO 13383-1:2016 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 13383-1:2016
EN ISO 13383-1:2016 (E)
European foreword
The text of ISO 13383-1:2012 has been prepared by Technical Committee ISO/TC 206 “Fine ceramics”
of the International Organization for Standardization (ISO) and has been taken over as EN
ISO 13383-1:2016 by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat
of which is held by DIN.
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 October 2016, and conflicting national standards shall
be withdrawn at the latest by October 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.
This document supersedes EN 623-3:2001.
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 13383-1:2012 has been approved by CEN as EN ISO 13383-1:2016 without any
modification.
3
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SIST EN ISO 13383-1:2016
INTERNATIONAL ISO
STANDARD 13383-1
First edition
2012-09-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Microstructural characterization —
Part 1:
Determination of grain size and size
distribution
Céramiques techniques — Caractérisation microstructurale —
Partie 1: Détermination de la grosseur du grain et de la distribution
granulométrique
Reference number
ISO 13383-1:2012(E)
©
ISO 2012
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SIST EN ISO 13383-1:2016
ISO 13383-1:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any
means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the
address below or ISO’s member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
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ISO 13383-1:2012(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Significance and use . 3
5 Apparatus . 4
5.1 Sectioning equipment . 4
5.2 Mounting equipment . 4
5.3 Grinding and polishing equipment . 4
5.4 Etching equipment. 4
5.5 Microscope . 4
5.6 Calibrated rule or scale . 5
5.7 Circle template . 5
6 Test piece preparation . 5
6.1 Sampling . 5
6.2 Cutting . 5
6.3 Mounting . 5
6.4 Grinding and polishing . 5
6.5 Etching . 6
7 Photomicrography . 6
7.1 General aspects . 6
7.2 Optical microscopy . 6
7.3 Scanning electron microscopy . 6
7.4 Calibration micrographs . 7
8 Measurement of micrographs . 7
8.1 General . 7
8.2 Method A1 . 8
8.3 Method A2 . 8
8.4 Method B . 8
8.5 Use of automatic or semi-automatic image analysis for methods A and B . 9
9 Calculation of results .10
9.1 Method A1 .10
9.2 Method A2 .10
9.3 Method B .10
10 Interferences and uncertainties .11
11 Test report .12
Annex A (informative) Grinding and polishing procedures .14
Annex B (informative) Etching procedures .16
Annex C (informative) Setting Köhler illumination in an optical microscope .18
Annex D (informative) Round-robin verification of Method A1.19
Annex E (informative) Round-robin verification of Method B .20
Annex F (informative) Grain size distribution measurement .21
Annex G (informative) Results sheet: Grain size in accordance with ISO 13383-1 .22
Bibliography .23
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ISO 13383-1:2012(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 13383-1 was prepared by Technical Committee ISO/TC 206, Fine ceramics.
ISO 13383 consists of the following parts, under the general title Fine ceramics (advanced ceramics,
advanced technical ceramics) — Microstructural characterization:
— Part 1: Determination of grain size and size distribution
— Part 2: Determination of phase volume fraction by evaluation of micrographs
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SIST EN ISO 13383-1:2016
INTERNATIONAL STANDARD ISO 13383-1:2012(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Microstructural characterization —
Part 1:
Determination of grain size and size distribution
1 Scope
This part of ISO 13383 describes manual methods of making measurements for the determination of
grain size of fine ceramics (advanced ceramics, advanced technical ceramics) using photomicrographs
of polished and etched test pieces. The methods described in this part do not yield the true mean grain
diameter, but a somewhat smaller parameter depending on the method applied to analyse a two-
dimensional section. The relationship to true grain dimensions depends on the grain shape and the
degree of microstructural anisotropy. This part contains two principal methods, A and B.
Method A is the mean linear intercept technique. Method A1 applies to single-phase ceramics, and to
ceramics with a principal crystalline phase and a glassy grain-boundary phase of less than about 5 % by
volume for which intercept counting suffices. Method A2 applies to ceramics with more than about 5 %
by volume of pores or secondary phases, or ceramics with more than one major crystalline phase where
individual intercept lengths are measured, which can optionally be used to create a size distribution.
This latter method allows the pores or phases to be distinguished and the mean linear intercept size for
each to be calculated separately.
NOTE A method of determining volume fraction(s) of secondary phase(s) can be found in ISO 13383:2; this
will provide a means of determining whether Method A1 or Method A2 should be applied in borderline cases.
Method B is the mean equivalent circle diameter method, which applies to any type of ceramic with or
without a secondary phase. This method may also be employed for determining grain aspect ratio and
a size distribution.
Some users of this part of ISO 13383 may wish to apply automatic or semiautomatic image analysis to
micrographs or directly captured microstructural images. This is permitted by this part provided that
the technique employed simulates the manual methods (see Clause 4 and 8.4).
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/IEC 17025, General requirements for the competence of testing and calibration laboratories
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
grain size
size of the distinct crystals in a material, and for the purposes of this method of test, that of the primary
or major phase
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3.2
mean linear intercept grain size
g
mli
average value of the distance between grain boundaries as shown by randomly positioned lines drawn
across a micrograph or other image of the microstructure
3.3
equivalent circle grain diameter
d
ci
diameter of a circle which closely matches the perimeter of a grain
See Figure 1.
3.4
maximum (Feret) grain size
d
ci, max
maximum dimension of a grain viewed in two dimensions
See Figure 1.
NOTE This is also termed maximum caliper diameter in ASTM E930.
3.5
maximum orthogonal grain size
d
ci, perp
for the purposes of determination of grain aspect ratio, the largest dimension of a grain normal to its
maximum (Feret) grain dimension, viewed in two dimensions
See Figure 1.
3.6
grain aspect ratio
ratio of maximum (Feret) grain size to the maximum orthogonal grain size measured perpendicular to it
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1
Key
1 Equivalent circle grain diameter, d
ci
2 Maximum grain (Feret) size, d
ci, max
3 Maximum orthogonal grain size perpendicular to 2, d
ci, perp
Figure 1 — Equivalent circle diameter and definition of aspect ratio
4 Significance and use
The mean grain size and the distribution of grain sizes of a ceramic material play an important role in
determining many properties, and thus grain size characterization is an important tool for ensuring
consistency of manufacture. There are many measures of grain size and/or shape, and these are usually
of different numerical values for a given microstructure.
NOTE The Bibliography contains sources dealing with stereology and methods of sizing three-
dimensional objects.
The principal purpose of this part of ISO 13383 is to permit characterization of the major phases.
However, in materials which contain more than one phase, the phases may be continuous or as isolated
grains. It may be necessary to characterize the different phases separately. The same intercept principle
as for single-phase materials can be used, but the individual intercept lengths across each phase must
be measured, rather than just counted. The characterization of minor phases may require different
treatment, which is outside the scope of this part of ISO 13383.
Method A, the linear intercept method, provides the simplest possible method from a two-dimensional
section through the material. However, it must be recognized that the numerical value obtained for
the mean linear intercept size is somewhat smaller than most other measures of grain size because
intercepts can cross grains at any position, and not necessarily along the largest axis. The relationship
between mean linear intercept size and a true three-dimensional grain size is not simple, and depends
on the grain shape and the average number of facets. This part of ISO 13383 provides simple methods of
measuring intercept distances in single-phase materials based on counting the number of intersections
along given lengths of randomly orientated and positioned lines or randomly positioned circles drawn
onto a micrograph of a suitably sectioned, polished and etched test piece. The length of lines crossing
large pores residing at grain boundaries can be ignored, thus eliminating any bias that porosity may
introduce, but small pores within grains should be ignored.
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Method B, the mean equivalent circle diameter method, provides an alternative approach based on
identifying the radius of a circle which most closely approximates the boundary of the grain. This
measure usually gives a result which is a little larger than that from the mean linear intercept method
because it is based on area and not random intercept length. The method may also be used to measure
grain aspect ratio, and is therefore more appropriate for microstructures with elongated grains.
[1]
NOTE This method is taken from JIS R1670 .
If the material possesses a microstructure which has a preferred orientation of the primary or
secondary phases, the results of this measurement may not be representative of the true character of
the material. Rather than using randomly orientated lines, it may be necessary to make measurements
restricted to specific orientations. If undertaken, this must be reported in the Test Report. Method B
may be more appropriate.
This part of ISO 13383 does not cover methods of measuring mean grain size by counting using calibrated
microscope stage movement or projection onto screens, accompanied by visual observation. While this
latter method may produce an equivalent result to the analysis of micrographs, it does not provide a
means of verification of the results of the measurement, since no permanent record is obtained.
If automatic or semiautomatic image analysis (AIA) is to be used, it must be recognized that different
AIA systems approach the measurement in different ways, usually based on pixel counting. In order
to obtain results equivalent to those of the manual methods described in this part of ISO 13383, the
AIA system needs to be programmed to operate in a similar way to the manual method. By agreement
between the parties concerned, such a near-equivalent AIA method may be used as an alternative to the
manual method, and if undertaken must be reported in the Test Report.
5 Apparatus
5.1 Sectioning equipment
A suitable fine-grained diamond-bladed cut-off saw with a liquid cooling or other device to prepare the
initial section for investigation.
[2]
NOTE A grit size of 125 µm to 150 µm is recommended, designated as D151 in ISO 6106 .
5.2 Mounting equipment
Suitable metallurgical mounting equipment and media for providing firm gripping of the test pieces
for polishing.
5.3 Grinding and polishing equipment
Suitable grinding and polishing equipment, employing diamond abrasive media.
NOTE Annex A recommends techniques and abrasives.
5.4 Etching equipment
Etching equipment appropriate to the etching process to be used to reveal grain boundaries in the
material being examined.
NOTE Annex B provides some guidelines for etching methods.
5.5 Microscope
An optical or scanning electron microscope with photomicrographic facilities. A calibrated stage
micrometer is required for determination of magnification in an optical microscope, and a reference
square grid or latex spheres are required for calibration of magnification in a scanning electron
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microscope. In all cases, the calibration of dimensions of the references shall be traceable to national or
international standards of length measurement.
An optical microscope is additionally required for assessing the quality of polishing (see 6.4).
5.6 Calibrated rule or scale
A calibrated rule or scale reading to 0,5 mm or better, and accurate to 0,5 % or better.
5.7 Circle template
For method B, a stencil cut with circles of diameter in 1 mm increments, or a transparent sheet with circles
drawn in a series of 1 mm increments. The line thickness on a transparent sheet shall not exceed 0,2 mm.
6 Test piece preparation
6.1 Sampling
The test pieces shall be sampled in a manner subject to agreement between the parties concerned.
NOTE Guidance on this issue may be found in EN 1006 (see Bibliography [3]). Depending on the objectives
of the measurement, it is desirable to maintain full knowledge of the positions within components or test pieces
from which sections are prepared.
6.2 Cutting
The required section of the test piece shall be cut using the sectioning device (see 5.1).
NOTE For routine inspection of materials, a small area of not more than 10 mm side is normally adequate as
the section to be polished.
6.3 Mounting
Mount the test piece using an appropriate mounting medium. If the ceramic is suspected to have
significant open porosity in some regions (see Clause 1), it is advisable to vacuum impregnate the test
piece with liquid mounting resin before encapsulating as this will provide some support during polishing.
NOTE It is not essential to encapsulate the test piece. For example, it could be affixed to a metal holder.
However, encapsulation in a polymer-based medium allows easy gripping and handling, especially of small
irregularly shaped test pieces and of weak, friable materials. The method of mounting selected should take into
account the etching procedure to be used; see Annex B.
6.4 Grinding and polishing
Grind and polish the surface of the test piece. Care should be taken to ensure that grinding produces
a planar surface with a minimum of damage. Employ successively smaller grit sizes, at each stage
removing the damage from the previous stage until there is no change in appearance when examined by
an optical microscope (see 5.5) at high magnification. The final surface shall be free from optically visible
scratches, or other damage introduced by polishing, which would interfere with the determination.
NOTE Care should be taken in choosing the sequence of grits and lap types. It is impossible within the scope
of this part of ISO 13383 to make specific recommendations for all types of material. The general principle to be
adopted is the minimization of subsurface damage, and its removal by progressively finer grits while retaining a
flat surface. Some guidelines on grinding and polishing are given in Annex A.
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ISO 13383-1:2012(E)
6.5 Etching
When a good quality surface has been achieved, the test piece shall be etched if necessary to reveal grain
boundaries. Any suitable technique appropriate to the ceramic ma
...
SLOVENSKI STANDARD
kSIST FprEN ISO 13383-1:2015
01-november-2015
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Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural
characterization - Part 1: Determination of grain size and size distribution (ISO 13383-
1:2012)
Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 1: Bestimmung der
Korngröße und der Korngrößenverteilung (ISO 13383-1:2012)
Céramiques techniques - Caractérisation microstructurale - Partie 1: Détermination de la
grosseur du grain et de la distribution granulométrique (ISO 13383-1:2012)
Ta slovenski standard je istoveten z: FprEN ISO 13383-1 rev
ICS:
81.060.30 Sodobna keramika Advanced ceramics
kSIST FprEN ISO 13383-1:2015 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST FprEN ISO 13383-1:2015
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kSIST FprEN ISO 13383-1:2015
EUROPEAN STANDARD
FINAL DRAFT
FprEN ISO 13383-1 rev
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2015
ICS 81.060.30 Will supersede EN 623-3:2001
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Microstructural characterization - Part 1:
Determination of grain size and size distribution (ISO 13383-
1:2012)
Céramiques techniques - Caractérisation microstructurale - Hochleistungskeramik - Mikrostrukturelle Charakterisierung
Partie 1: Détermination de la grosseur du grain et de la - Teil 1: Bestimmung der Korngröße und der
distribution granulométrique (ISO 13383-1:2012) Korngrößenverteilung (ISO 13383-1:2012)
This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical
Committee CEN/TC 184.
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-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.
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.
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.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprEN ISO 13383-1 rev:2015 E
worldwide for CEN national Members.
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FprEN ISO 13383-1:2015 (E)
Contents Page
European foreword .3
2
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kSIST FprEN ISO 13383-1:2015
FprEN ISO 13383-1:2015 (E)
European foreword
The text of ISO 13383-1:2012 has been prepared by Technical Committee ISO/TC 206 “Fine ceramics” of the
International Organization for Standardization (ISO) and has been taken over as FprEN ISO 13383-1:2015 by
Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by DIN.
This document is currently submitted to the Unique Acceptance Procedure.
This document will supersede EN 623-3:2001.
Endorsement notice
The text of ISO 13383-1:2012 has been approved by CEN as FprEN ISO 13383-1:2015 without any
modification.
3
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kSIST FprEN ISO 13383-1:2015
INTERNATIONAL ISO
STANDARD 13383-1
First edition
2012-09-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Microstructural characterization —
Part 1:
Determination of grain size and size
distribution
Céramiques techniques — Caractérisation microstructurale —
Partie 1: Détermination de la grosseur du grain et de la distribution
granulométrique
Reference number
ISO 13383-1:2012(E)
©
ISO 2012
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kSIST FprEN ISO 13383-1:2015
ISO 13383-1:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any
means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the
address below or ISO’s member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
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Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Significance and use . 3
5 Apparatus . 4
5.1 Sectioning equipment . 4
5.2 Mounting equipment . 4
5.3 Grinding and polishing equipment . 4
5.4 Etching equipment. 4
5.5 Microscope . 4
5.6 Calibrated rule or scale . 5
5.7 Circle template . 5
6 Test piece preparation . 5
6.1 Sampling . 5
6.2 Cutting . 5
6.3 Mounting . 5
6.4 Grinding and polishing . 5
6.5 Etching . 6
7 Photomicrography . 6
7.1 General aspects . 6
7.2 Optical microscopy . 6
7.3 Scanning electron microscopy . 6
7.4 Calibration micrographs . 7
8 Measurement of micrographs . 7
8.1 General . 7
8.2 Method A1 . 8
8.3 Method A2 . 8
8.4 Method B . 8
8.5 Use of automatic or semi-automatic image analysis for methods A and B . 9
9 Calculation of results .10
9.1 Method A1 .10
9.2 Method A2 .10
9.3 Method B .10
10 Interferences and uncertainties .11
11 Test report .12
Annex A (informative) Grinding and polishing procedures .14
Annex B (informative) Etching procedures .16
Annex C (informative) Setting Köhler illumination in an optical microscope .18
Annex D (informative) Round-robin verification of Method A1.19
Annex E (informative) Round-robin verification of Method B .20
Annex F (informative) Grain size distribution measurement .21
Annex G (informative) Results sheet: Grain size in accordance with ISO 13383-1 .22
Bibliography .23
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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 13383-1 was prepared by Technical Committee ISO/TC 206, Fine ceramics.
ISO 13383 consists of the following parts, under the general title Fine ceramics (advanced ceramics,
advanced technical ceramics) — Microstructural characterization:
— Part 1: Determination of grain size and size distribution
— Part 2: Determination of phase volume fraction by evaluation of micrographs
iv © ISO 2012 – All rights reserved
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kSIST FprEN ISO 13383-1:2015
INTERNATIONAL STANDARD ISO 13383-1:2012(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Microstructural characterization —
Part 1:
Determination of grain size and size distribution
1 Scope
This part of ISO 13383 describes manual methods of making measurements for the determination of
grain size of fine ceramics (advanced ceramics, advanced technical ceramics) using photomicrographs
of polished and etched test pieces. The methods described in this part do not yield the true mean grain
diameter, but a somewhat smaller parameter depending on the method applied to analyse a two-
dimensional section. The relationship to true grain dimensions depends on the grain shape and the
degree of microstructural anisotropy. This part contains two principal methods, A and B.
Method A is the mean linear intercept technique. Method A1 applies to single-phase ceramics, and to
ceramics with a principal crystalline phase and a glassy grain-boundary phase of less than about 5 % by
volume for which intercept counting suffices. Method A2 applies to ceramics with more than about 5 %
by volume of pores or secondary phases, or ceramics with more than one major crystalline phase where
individual intercept lengths are measured, which can optionally be used to create a size distribution.
This latter method allows the pores or phases to be distinguished and the mean linear intercept size for
each to be calculated separately.
NOTE A method of determining volume fraction(s) of secondary phase(s) can be found in ISO 13383:2; this
will provide a means of determining whether Method A1 or Method A2 should be applied in borderline cases.
Method B is the mean equivalent circle diameter method, which applies to any type of ceramic with or
without a secondary phase. This method may also be employed for determining grain aspect ratio and
a size distribution.
Some users of this part of ISO 13383 may wish to apply automatic or semiautomatic image analysis to
micrographs or directly captured microstructural images. This is permitted by this part provided that
the technique employed simulates the manual methods (see Clause 4 and 8.4).
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/IEC 17025, General requirements for the competence of testing and calibration laboratories
3 Terms a nd definiti ons
For the purposes of this document, the following terms and definitions apply.
3.1
grain size
size of the distinct crystals in a material, and for the purposes of this method of test, that of the primary
or major phase
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3.2
mean linear intercept grain size
g
mli
average value of the distance between grain boundaries as shown by randomly positioned lines drawn
across a micrograph or other image of the microstructure
3.3
equivalent circle grain diameter
d
ci
diameter of a circle which closely matches the perimeter of a grain
See Figure 1.
3.4
maximum (Feret) grain size
d
ci, max
maximum dimension of a grain viewed in two dimensions
See Figure 1.
NOTE This is also termed maximum caliper diameter in ASTM E930.
3.5
maximum orthogonal grain size
d
ci, perp
for the purposes of determination of grain aspect ratio, the largest dimension of a grain normal to its
maximum (Feret) grain dimension, viewed in two dimensions
See Figure 1.
3.6
grain aspect ratio
ratio of maximum (Feret) grain size to the maximum orthogonal grain size measured perpendicular to it
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2
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1
Key
1 Equivalent circle grain diameter, d
ci
2 Maximum grain (Feret) size, d
ci, max
3 Maximum orthogonal grain size perpendicular to 2, d
ci, perp
F i g u r e 1 — E qu i v a lent c i r c le d i a me t er a nd de f i n it ion of a s p e c t r at io
4 Sig nificance and use
The mean grain size and the distribution of grain sizes of a ceramic material play an important role in
determining many properties, and thus grain size characterization is an important tool for ensuring
consistency of manufacture. There are many measures of grain size and/or shape, and these are usually
of different numerical values for a given microstructure.
NOTE The Bibliography contains sources dealing with stereology and methods of sizing three-
dimensional objects.
The principal purpose of this part of ISO 13383 is to permit characterization of the major phases.
However, in materials which contain more than one phase, the phases may be continuous or as isolated
grains. It may be necessary to characterize the different phases separately. The same intercept principle
as for single-phase materials can be used, but the individual intercept lengths across each phase must
be measured, rather than just counted. The characterization of minor phases may require different
treatment, which is outside the scope of this part of ISO 13383.
Method A, the linear intercept method, provides the simplest possible method from a two-dimensional
section through the material. However, it must be recognized that the numerical value obtained for
the mean linear intercept size is somewhat smaller than most other measures of grain size because
intercepts can cross grains at any position, and not necessarily along the largest axis. The relationship
between mean linear intercept size and a true three-dimensional grain size is not simple, and depends
on the grain shape and the average number of facets. This part of ISO 13383 provides simple methods of
measuring intercept distances in single-phase materials based on counting the number of intersections
along given lengths of randomly orientated and positioned lines or randomly positioned circles drawn
onto a micrograph of a suitably sectioned, polished and etched test piece. The length of lines crossing
large pores residing at grain boundaries can be ignored, thus eliminating any bias that porosity may
introduce, but small pores within grains should be ignored.
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Method B, the mean equivalent circle diameter method, provides an alternative approach based on
identifying the radius of a circle which most closely approximates the boundary of the grain. This
measure usually gives a result which is a little larger than that from the mean linear intercept method
because it is based on area and not random intercept length. The method may also be used to measure
grain aspect ratio, and is therefore more appropriate for microstructures with elongated grains.
[1]
NOTE This method is taken from JIS R1670 .
If the material possesses a microstructure which has a preferred orientation of the primary or
secondary phases, the results of this measurement may not be representative of the true character of
the material. Rather than using randomly orientated lines, it may be necessary to make measurements
restricted to specific orientations. If undertaken, this must be reported in the Test Report. Method B
may be more appropriate.
This part of ISO 13383 does not cover methods of measuring mean grain size by counting using calibrated
microscope stage movement or projection onto screens, accompanied by visual observation. While this
latter method may produce an equivalent result to the analysis of micrographs, it does not provide a
means of verification of the results of the measurement, since no permanent record is obtained.
If automatic or semiautomatic image analysis (AIA) is to be used, it must be recognized that different
AIA systems approach the measurement in different ways, usually based on pixel counting. In order
to obtain results equivalent to those of the manual methods described in this part of ISO 13383, the
AIA system needs to be programmed to operate in a similar way to the manual method. By agreement
between the parties concerned, such a near-equivalent AIA method may be used as an alternative to the
manual method, and if undertaken must be reported in the Test Report.
5 Apparatus
5.1 Sectioning equipment
A suitable fine-grained diamond-bladed cut-off saw with a liquid cooling or other device to prepare the
initial section for investigation.
[2]
NOTE A grit size of 125 µm to 150 µm is recommended, designated as D151 in ISO 6106 .
5.2 Mounting equipment
Suitable metallurgical mounting equipment and media for providing firm gripping of the test pieces
for polishing.
5.3 Grinding and polishing equipment
Suitable grinding and polishing equipment, employing diamond abrasive media.
NOTE Annex A recommends techniques and abrasives.
5.4 Etching equipment
Etching equipment appropriate to the etching process to be used to reveal grain boundaries in the
material being examined.
NOTE Annex B provides some guidelines for etching methods.
5.5 Microscope
An optical or scanning electron microscope with photomicrographic facilities. A calibrated stage
micrometer is required for determination of magnification in an optical microscope, and a reference
square grid or latex spheres are required for calibration of magnification in a scanning electron
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microscope. In all cases, the calibration of dimensions of the references shall be traceable to national or
international standards of length measurement.
An optical microscope is additionally required for assessing the quality of polishing (see 6.4).
5.6 Calibrated rule or scale
A calibrated rule or scale reading to 0,5 mm or better, and accurate to 0,5 % or better.
5.7 Circle template
For method B, a stencil cut with circles of diameter in 1 mm increments, or a transparent sheet with circles
drawn in a series of 1 mm increments. The line thickness on a transparent sheet shall not exceed 0,2 mm.
6 Test piece preparation
6.1 Sampling
The test pieces shall be sampled in a manner subject to agreement between the parties concerned.
NOTE Guidance on this issue may be found in EN 1006 (see Bibliography [3]). Depending on the objectives
of the measurement, it is desirable to maintain full knowledge of the positions within components or test pieces
from which sections are prepared.
6.2 Cutting
The required section of the test piece shall be cut using the sectioning device (see 5.1).
NOTE For routine inspection of materials, a small area of not more than 10 mm side is normally adequate as
the section to be polished.
6.3 Mounting
Mount the test piece using an appropriate mounting medium. If the ceramic is suspected to have
significant open porosity in some regions (see Clause 1), it is advisable to vacuum impregnate the test
piece with liquid mounting resin before encapsulating as this will provide some support during polishing.
NOTE It is not essential to encapsulate the test piece. For example, it could be affixed to a metal holder.
However, encapsulation in a polymer-based medium allows easy gripping and handling, especially of small
irregularly shaped test pieces and of weak, friable materials. The method of mounting selected should take into
account the etching procedure to be used; see Annex B.
6.4 Grinding and polishing
Grind and polish the surface of the test piece. Care should be taken to ensure that grinding produces
a planar surface with a minimum of damage. Employ successively smaller grit sizes, at each stage
removing the damage from the previous stage until there is no change in appearance when examined by
an optical microscope (see 5.5) at high magnification. The final surface shall be free from optically visible
scratches, or other damage introduced by polishing, which would interfere with the determination.
NOTE Care should be taken in choosing the sequence of grits and lap types. It is impossible within the scope
of this part of ISO 13383 to make specific recommendations for all types of material. The general principle to be
adopted is the minimization of subsurface damage, and its removal by progressively finer grits while retaining a
flat surface. Some guidelines on grinding and polishing are given in Annex A.
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6.5 Etching
When a good quality surface has been achieved, the test piece shall be etched if necessary to reveal grain
boundaries. Any suitable technique appropriate to the ceramic material class shall be used, subject to
agreement between the parties concerned. Excessive intensity of etching shall be avoided.
NOTE Some general guidelines recommending etching procedures for various commonly available advanced
technical ceramics are given in Annex B.
7 Photomicrography
7.1 General aspects
Either optical microscopy or scanning electron microscopy may be used, the latter being required if the
grain structure is on a sca
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