SIST EN ISO 13383-2:2016

Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural characterization - Part 2: Determination of phase volume fraction by evaluation of micrographs (ISO 13383-2:2012)

This part of ISO 13383 specifies a manual method of making measurements for the determination of the volume fraction of major phases in fine ceramics (advanced ceramics, advanced technical ceramics) using micrographs of polished and etched sections, overlaying a square grid of lines, and counting the number of intersections lying over each phase.

Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 2: Bestimmung des Volumenanteils von Phasen durch Auswertung von Mikrogefügeaufnahmen (ISO 13383-2:2012)

Dieser Teil von ISO 13383 legt ein manuelles Messverfahren zur Bestimmung des Volumenanteils der Hauptphasen in Hochleistungskeramiken fest, in dem auf Mikroaufnahmen polierter und geätzter Querschnitte ein quadratisches Liniengitter aufgelegt und die Anzahl der Schnittpunkte der Gitterlinien über jeder Phase ausgezählt wird.
ANMERKUNG 1 Bei diesem Verfahren wird vorausgesetzt, dass die tatsächlich vorhandenen Volumenanteile einer Phase nach stereologischen Prinzipien den Flächenanteilen entsprechen, die auf einem zufällig festgelegten Querschnitt vorhanden sind.
ANMERKUNG 2 Anleitungen zum Polieren und Ätzen von Hochleistungskeramiken können ISO 13383-1:2012, Anhänge A und B, entnommen werden.
Das Verfahren gilt für keramische Werkstoffe mit einer oder mehreren deutlich erkennbaren Sekundärphasen, die z. B. in Al2O3/ZrO2, Si/SiC oder in Al2O3/SiCw zu finden sind.
Falls das Prüfmaterial diskrete Poren enthält, können sie im Rahmen dieses Verfahrens als Sekundärphase angesehen werden, sofern es keine Hinweise darauf gibt, dass beim Polieren Körner herausgebrochen wurden, die mit echten Poren verwechselt werden könnten.
ANMERKUNG 3 Falls der Werkstoff eine Porosität von mehr als etwa 20 % aufweist, besteht ein großes Risiko, dass beim Polieren eine Beschädigung des Mikrogefüges auftritt und die Messung des Porenvolumenanteils irreführend sein kann. Ergebnisse der Bestimmung von Volumenanteilen einer Sekundärphase oder von Porenvolumenanteilen, die weniger als 0,05 betragen, können merkliche Fehler und möglicherweise auch eine Streuung aufweisen. Um die Konsistenz und Genauigkeit der Ergebnisse zu verbessern, muss normalerweise eine größere Anzahl als die übliche Anzahl von mindestens drei Mikroaufnahmen ausgewertet werden.

Céramiques techniques - Caractérisation microstructurale - Partie 2: Détermination de la fraction volumique des phases par évaluation de micrographes (ISO 13383-2:2012)

L'ISO 13383-2:2012 spécifie une méthode manuelle de mesurage en vue de la détermination de la fraction volumique des phases principales de céramiques techniques en utilisant des micrographies de sections polies et soumises à une attaque, en les recouvrant d'un quadrillage carré et en comptant le nombre d'intersections situées au-dessus de chaque phase.
La méthode s'applique aux céramiques comportant une ou plusieurs phases secondaires distinctes, telles que celles rencontrées dans Al2O3/ZrO2, Si/SiC ou Al2O3/SiCw.
Si le matériau d'essai contient des pores discrets, ceux-ci doivent être traités comme une phase secondaire pour les besoins de la présente méthode, à condition qu'il n'y ait aucun signe d'arrachement des grains pendant le polissage pouvant être confondu avec des pores authentiques.

Fina keramika (sodobna keramika, sodobna tehnična keramika) - Značilnosti mikrostrukture - 2. del: Določanje volumenskega deleža faz z vrednotenjem mikrostrukture (ISO 13383-2:2012)

Ta del standarda ISO 13383 opredeljuje ročno metodo izvajanja meritev za določanje volumenskega deleža glavnih faz v fini keramiki (sodobni keramiki, sodobni tehnični keramiki) z mikrografi poliranih in jedkanih delov, tako da se prek njih položi kvadratna mreža črt in se prešteje število presekov, ki ležijo nad posamezno fazo.

General Information

• Status: Published
• Public Enquiry End Date: 29-Nov-2015
• Publication Date: 16-May-2016
• ICS: 81.060.30 - Advanced ceramics
• Technical Committee: I13 - Imaginarni 13
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 06-May-2016
• Due Date: 11-Jul-2016
• Completion Date: 17-May-2016
• Ref Project: EN ISO 13383-2:2016 - Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural characterization - Part 2: Determination of phase volume fraction by evaluation of micrographs (ISO 13383-2:2012)

Relations

• Replaces: SIST EN 623-5:2009 - Advanced technical ceramics - Monolithic ceramics - General and textural properties - Part 5: Determination of phase volume fraction by evaluation of micrographs
• Effective Date: 01-Jun-2016

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 13383-2:2016
01-junij-2016
1DGRPHãþD
SIST EN 623-5:2009
)LQDNHUDPLNDVRGREQDNHUDPLNDVRGREQDWHKQLþQDNHUDPLND=QDþLOQRVWL
PLNURVWUXNWXUHGHO'RORþDQMHYROXPHQVNHJDGHOHåDID]]YUHGQRWHQMHP
PLNURVWUXNWXUH,62
Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural
characterization - Part 2: Determination of phase volume fraction by evaluation of
micrographs (ISO 13383-2:2012)
Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 2: Bestimmung des
Volumenanteils von Phasen durch Auswertung von Mikrogefügeaufnahmen (ISO 13383-
2:2012)
Céramiques techniques - Caractérisation microstructurale - Partie 2: Détermination de la
fraction volumique des phases par évaluation de micrographes (ISO 13383-2:2012)
Ta slovenski standard je istoveten z: EN ISO 13383-2:2016
ICS:
81.060.30 Sodobna keramika Advanced ceramics
SIST EN ISO 13383-2:2016 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13383-2:2016

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SIST EN ISO 13383-2:2016


EN ISO 13383-2
EUROPEAN STANDARD

NORME EUROPÉENNE

April 2016
EUROPÄISCHE NORM
ICS 81.060.30 Supersedes EN 623-5:2009
English Version

Fine ceramics (advanced ceramics, advanced technical
ceramics) - Microstructural characterization - Part 2:
Determination of phase volume fraction by evaluation of
micrographs (ISO 13383-2:2012)
Céramiques techniques - Caractérisation Hochleistungskeramik - Mikrostrukturelle
microstructurale - Partie 2: Détermination de la Charakterisierung - Teil 2: Bestimmung des
fraction volumique des phases par évaluation de Volumenanteils von Phasen durch Auswertung von
micrographies (ISO 13383-2:2012) Mikrogefügeaufnahmen (ISO 13383-2:2012)
This European Standard was approved by CEN on 19 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 13383-2:2016 E
worldwide for CEN national Members.

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SIST EN ISO 13383-2:2016
EN ISO 13383-2:2016 (E)
Contents Page
European foreword . 3
2

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SIST EN ISO 13383-2:2016
EN ISO 13383-2:2016 (E)
European foreword
The text of ISO 13383-2:2012 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 13383-2:2016 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 623-5:2009.
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 13383-2:2012 has been approved by CEN as EN ISO 13383-2:2016 without any
modification.


3

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SIST EN ISO 13383-2:2016

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SIST EN ISO 13383-2:2016
INTERNATIONAL ISO
STANDARD 13383-2
First edition
2012-09-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Microstructural characterization —
Part 2:
Determination of phase volume
fraction by evaluation of micrographs
Céramiques techniques — Caractérisation microstructurale —
Partie 2: Détermination de la fraction volumique des phases par
évaluation de micrographes
Reference number
ISO 13383-2:2012(E)
©
ISO 2012

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(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 [e-mail]
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Apparatus . 2
4.1 Sectioning equipment . 2
4.2 Mounting equipment . 2
4.3 Grinding and polishing equipment . 2
4.4 Microscope . 2
4.5 Transparent grid . 2
5 Test piece preparation . 3
5.1 Sampling . 3
5.2 Cutting . 3
5.3 Mounting . 3
5.4 Grinding and polishing . 3
5.5 Etching . 3
6 Photomicrography . 4
6.1 General aspects . 4
6.2 Inspection . 4
6.3 Number of micrographs . 4
6.4 Optical microscopy . 4
6.5 Scanning electron microscopy . 5
7 Measurement of micrographs . 5
8 Calculation of results . 6
9 Interferences and uncertainties . 6
10 Test report . 7
Annex A (informative) Use of automatic image analysis (AIA). 9
Annex B (informative) Round-robin verification of this procedure .10
Annex C (informative) Results sheet — ISO 13383-2 .11
Bibliography .12
© ISO 2012 – All rights reserved iii

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(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.
ISO 13383-2 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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SIST EN ISO 13383-2:2016
INTERNATIONAL STANDARD ISO 13383-2:2012(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Microstructural characterization —
Part 2:
Determination of phase volume fraction by evaluation of
micrographs
1 Scope
This part of ISO 13383 specifies a manual method of making measurements for the determination of
the volume fraction of major phases in fine ceramics (advanced ceramics, advanced technical ceramics)
using micrographs of polished and etched sections, overlaying a square grid of lines, and counting the
number of intersections lying over each phase.
NOTE 1 This method assumes that the true phase volume fractions are equivalent to area fractions on a
randomly cut cross-section according to stereological principles.
NOTE 2 Guidelines for polishing and etching of advanced technical ceramics can be found in Annexes A and B
of ISO 13383-1:2012.
The method applies to ceramics with one or more distinct secondary phases, such as found in Al O /ZrO ,
2 3 2
Si/SiC, or Al O /SiC .
2 3 w
If the test material contains discrete pores, these are to be treated as a secondary phase for the purpose
of this method, provided that there is no evidence of grain pluck-out during polishing being confused
with genuine pores.
NOTE 3 If the material contains more than about 20 % porosity, there is a strong risk that the microstructure
will be damaged during the polishing process, and measurement of the volume fraction of pores may become
misleading. Secondary phase volume fractions or porosity present at levels of less than 0,05 are subject to
considerable error and potential scatter in results. A larger number of micrographs than the minimum of three is
normally needed to improve the consistency and accuracy of the results.
NOTE 4 Many ceramics contain small amounts of secondary glassy phases. In order to make a reasonable
estimate of glassy phase content, the glass material between crystalline grains should be readily observable, and
thus should be at least 0,5 µm in width. The method in this part of ISO 13383 is not considered appropriate for
narrow glassy films around grains.
NOTE 5 Microstructures are seldom homogeneous, and the phase contents can vary from micrograph to
micrograph. It is essential to survey a sufficiently wide area of the prepared section to ensure that those areas
selected for evaluation are representative, and do not contain eye-catching irregularities. This method assumes
that the selected regions of a prepared cross-section are statistically representative of the whole sampled section.
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 currently outside the scope of this
part, but some guidelines are given in Annex A.
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
© ISO 2012 – All rights reserved 1

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(E)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
phase volume fraction
volume occupied by a distinct, identifiable phase present in a material expressed as a fraction of the whole
3.2
primary phase
principal phase within a microstructure, typically comprising more than 50 % by volume or observed
area in a cross-section
3.3
secondary phase
one or more distinct identifiable phases other than a primary crystalline phase in a material
NOTE A secondary phase can be in the form of discrete grains, or as a continuous phase surrounding some or all of
the major phase grains. For the purposes of this part of ISO 13383, porosity may be treated as a secondary phase.
4 Apparatus
4.1 Sectioning equipment
Any suitable method may be used for preparing the test section from the item under investigation. If a
diamond-bladed cut-off saw is employed, it is recommended that the grit size should not exceed 150 µm.
[5]
NOTE This grit size is designated as D151 according to ISO 6106 .
4.2 Mounting equipment
Suitable metallurgical mounting equipment and media for providing firm gripping of the test piece
for polishing.
4.3 Grinding and polishing equipment
Suitable grinding and polishing equipment, employing diamond abrasive media.
NOTE A sequence of abrasives and techniques recommended for polishing are given in Annex A of
ISO 13383-1:2012.
4.4 Microscope
An optical or scanning electron microscope with photomicrographic facilities.
NOTE Although the true magnification of the image is unimportant for making the measurement of the
volume fraction, it is advised that a reference graticule may be used to determine magnification in an optical
microscope, or a reference grid or latex spheres may be used for calibration of magnification in a scanning electron
microscope, and as a check on the homogeneity of magnification across the field of view.
An optical microscope is additionally required for assessing the quality of polishing (see 5.4).
4.5 Transparent grid
Transparent square grid on, e.g. acetate film, and with line thickness not exceeding 0,1 mm.
NOTE 1 The grid spacing selected is not critical, but may conveniently be between 3 mm and 15 mm to minimize
eyestrain. However, it is necessary that consideration of the requirements of 6.3 is taken into account.
2 © ISO 2012 – All rights reserved

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(E)
NOTE 2 A suitable grid may be prepared as a computer plot with sufficient accuracy of line spacing for the
purposes of this part of ISO 13383.
5 Test piece preparation
5.1 Sampling
The test pieces shall be sampled in a manner subject to agreement between parties.
NOTE Guidance on this issue may be found in EN 1006 (see Bibliography [18]). Depending on the objectives
of performing the measurement, it is desirable to maintain knowledge of the positions within components or test
pieces from which sections are prepared.
5.2 Cutting
The required section of test piece shall be cut using the sectioning equipment (see 4.1).
NOTE For routine inspection of materials, a small area of side no more than 10 mm is normally adequate as
the section to be polished.
5.3 Mounting
Mount the test piece using an appropriate mounting medium.
NOTE 1 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 grinding and polishing.
NOTE 2 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 test pieces. The method of mounting selected should take into
account the etching procedure to be used; see Annex B.
5.4 Grinding and polishing
Grind and polish the surface of the test piece. Care shall 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 4.4) at high magnification. At least 90 % of the test piece area shall be
free from optically visible scratches, or other damage introduced by polishing, which will interfere with
the determination. In particular, avoid the plucking out of discrete secondary phases from the surface
giving the appearance of pores.
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 polishing are given in Annex A of ISO 13383-1:2012.
5.5 Etching
When a good quality polished surface has been achieved, the test piece shall be etched if necessary to
reveal the individual phases. Any suitable technique shall be used, subject to agreement between parties.
NOTE 1 Some general guidelines recommending etching procedures for various commonly available advanced
technical ceramics are given in Annex B of ISO 13383-1:2012.
© ISO 2012 – All rights reserved 3

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(E)
NOTE 2 For optical evaluation, it is usually necessary to etch oxide materials in such a way that the individual
phases are distinguished by having different contrast levels. For scanning electron microscope (SEM) evaluation,
it may not be necessary to etch if a backscattered electron detector is used which has adequate resolution of net
atomic number difference between the phases such that contrast is generated. If a secondary electron detector
is used, it will usually be necessary to etch to produce topographic contrast unless the atomic number difference
between the phases is large.
6 Photomicrography
6.1 General aspects
If it is found that the average grain size of each phase or the widths of continuous glassy phases between
grains is less than 2 µm, prepare the test piece for scanning electron microscopy. For grain sizes between
2 µm and 4 µm, either scanning electron microscopy or optical microscopy are permitted. Otherwise,
optical microscopy is adequate.
It is important to achieve sufficient contrast between phases in order to identify individual grains clearly
and unambiguously.
6.2 Inspection
Inspect the sampled cross-section in the microscope. If the microstructure appears homogeneous,
prepare micrographs from randomly selected areas.
NOTE If inhomogeneity of microstructure is suspected or specific regions of a section need to be investigated,
this is permitted but must be reported in the report.
6.3 Number of micrographs
At least three micrographs shall be prepared at a magnification sufficient to identify clearly all the
phases to be counted. In addition, at least 100 features in total of any given type shall be present to be
counted in the set of micrographs.
NOTE For a nominally homogeneous material, it may be sufficient to use a small number of micrographs
analysed with a small grid spacing, but for an inhomogeneous material, results representative of the average for
the sampled section can be prepared reliably only by selecting a large number of micrographs of different areas,
with less intensive counting from a larger grid.
6.4 Optical microscopy
Set up Köhler illumination in the microscope.
NOTE 1 Guidance on setting Köhler illumination conditions is given in Annex D of ISO 13383-1:2012.
Examine the test piece at a magnification sufficient to resolve the individual grains clearly. If the contrast
obtained is insufficient, e.g. in white or translucent materials, apply a suitable thin metallic coating by
evaporation or sputtering.
Prepare micrographs of at least three different randomly selected areas of the test-piece surface, taking
into account the apparent homogeneity of the microstructure (see 6.2).
NOTE 2 As a guideline, the average size of discrete phase area to be counted should appear typically at least
3 mm across. If the total number of individual grains of any one phase to be counted in any one set of micrographs
is less than one hundred, prepare more micrographs. Micrographs should be typically of a size 100 mm x 75 mm,
but may with advantage be enlarged later to aid evaluation.
4 © ISO 2012 – All rights reserved

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(E)
6.5 Scanning electron microscopy
Mount the test piece on the test piece holder of the microscope. If the test piece is not electrically
conducting, apply a thin evaporated or sputtered conductive coating. Insert the test-piece in the
microscope, ensuring that the surface to be characterized is normal to the electron beam to within 5°.
NOTE 1 This ensures that the image does not suffer from excessive distortion or loss of focus due to the
angle of viewing.
Prepare micrographs at a suitable magnification (see 6.4) from at least three different randomly selected
areas of the test piece, using either secondary electron imaging or backscattered electron imaging.
NOTE 2 Although the contrast between phases can be enhanced using backscattered electron imaging, a
noisier image than in secondary electron imaging may result and may render the boundaries between contrasting
phases indistinct. It can be helpful to use secondary electron images for counting the phase proportions, but
backscattered images to aid identification of each phase.
If the number of grains of the phase to be counted is less than 100 in total over all the micrographs,
increase the number of areas photographed. Micrographs shall be typically be of a size 100 mm x 75 mm,
but may with advantage be enlarged later to aid evaluation.
NOTE 3 It is possible that the photographic screen in the microscope will not have constant magnification at
all points. A square grid makes a suitable reference for ascertaining the degree of distortion in the screen, since
it is easy to detect distortions of the grid. For the purposes of this test method, distortions of typically up to 5 %
may be acceptable provided that the phases being counted are distributed homogeneously across the entire area
of the micrograph.
7 Measurement of micrographs
If desirable, enlarge the photomicrograph to a size suitable for easier observation of the features.
Examine the dimensions of the smallest features to be counted. Select a suitable grid spacing and
prepare a square grid (see 4.5, 6.3 and Clause 9) such that the grid area covers the entire micrograph.
Tape the micrograph to a smooth surface. Overlay the grid such that the entire area of the micrograph is
covered by the grid, with no grid intersections immediately over the edges of the micrograph (Figure 1).
Count the number of grid intersections n of the grid that lie over each phase j. If the grid intersection
ij
lies exactly over the boundary between two phases, count this as one-half of a grid intersection for each
phase. If porosity is to be estimated, use the same rule for when a grid intersection lies exactly on the
edge of a pore. Count the total number of grid intersections over the area of the micrograph. If pores are
not being counted, count the number of grid intersections lying over the crystalline or glassy phases in
the material.
NOTE It can be helpful in counting to screen with pieces of paper those lines of intersections above and below
the one being counted; this reduces eye strain and the risk of miscounting, as shown in Figure 1.
© ISO 2012 – All rights reserved 5

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SIST EN ISO 13383-2:2016
ISO 13383-2:2012(E)
Figure 1 — Schematic diagram of microstructure overlaid with s
...

SLOVENSKI STANDARD
kSIST FprEN ISO 13383-2:2015
01-november-2015
)LQDNHUDPLNDVRGREQDNHUDPLNDVRGREQDWHKQLþQDNHUDPLND=QDþLOQRVWL
PLNURVWUXNWXUHGHO'RORþDQMHYROXPHQVNHJDGHOHåDID]]YUHGQRWHQMHP
PLNURVWUXNWXUH,62
Fine ceramics (advanced ceramics, advanced technical ceramics) - Microstructural
characterization - Part 2: Determination of phase volume fraction by evaluation of
micrographs (ISO 13383-2:2012)
Hochleistungskeramik - Mikrostrukturelle Charakterisierung - Teil 2: Bestimmung des
Volumenanteils von Phasen durch Auswertung von Mikrogefügeaufnahmen (ISO 13383-
2:2012)
Céramiques techniques - Caractérisation microstructurale - Partie 2: Détermination de la
fraction volumique des phases par évaluation de micrographes (ISO 13383-2:2012)
Ta slovenski standard je istoveten z: FprEN ISO 13383-2 rev
ICS:
81.060.30 Sodobna keramika Advanced ceramics
kSIST FprEN ISO 13383-2:2015 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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kSIST FprEN ISO 13383-2:2015

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kSIST FprEN ISO 13383-2:2015

EUROPEAN STANDARD
FINAL DRAFT
FprEN ISO 13383-2 rev
NORME EUROPÉENNE

EUROPÄISCHE NORM

September 2015
ICS 81.060.30 Will supersede EN 623-5:2009
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Microstructural characterization - Part 2:
Determination of phase volume fraction by evaluation of
micrographs (ISO 13383-2:2012)
Céramiques techniques - Caractérisation microstructurale - Hochleistungskeramik - Mikrostrukturelle Charakterisierung
Partie 2: Détermination de la fraction volumique des phases - Teil 2: Bestimmung des Volumenanteils von Phasen durch
par évaluation de micrographes (ISO 13383-2:2012) Auswertung von Mikrogefügeaufnahmen (ISO 13383-
2:2012)
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,
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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 13383-2 rev:2015 E
worldwide for CEN national Members.

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kSIST FprEN ISO 13383-2:2015
FprEN ISO 13383-2:2015 (E)
Contents Page
European foreword .3
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kSIST FprEN ISO 13383-2:2015
FprEN ISO 13383-2:2015 (E)
European foreword
The text of ISO 13383-2:2012 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 13383-2:2015 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 623-5:2009.
Endorsement notice
The text of ISO 13383-2:2012 has been approved by CEN as FprEN ISO 13383-2:2015 without any
modification.
3

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kSIST FprEN ISO 13383-2:2015

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kSIST FprEN ISO 13383-2:2015
INTERNATIONAL ISO
STANDARD 13383-2
First edition
2012-09-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Microstructural characterization —
Part 2:
Determination of phase volume
fraction by evaluation of micrographs
Céramiques techniques — Caractérisation microstructurale —
Partie 2: Détermination de la fraction volumique des phases par
évaluation de micrographes
Reference number
ISO 13383-2:2012(E)
©
ISO 2012

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kSIST FprEN ISO 13383-2:2015
ISO 13383-2:2012(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
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Tel. + 41 22 749 01 11
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Published in Switzerland
ii © ISO 2012 – All rights reserved

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kSIST FprEN ISO 13383-2:2015
ISO 13383-2:2012(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Apparatus . 2
4.1 Sectioning equipment . 2
4.2 Mounting equipment . 2
4.3 Grinding and polishing equipment . 2
4.4 Microscope . 2
4.5 Transparent grid . 2
5 Test piece preparation . 3
5.1 Sampling . 3
5.2 Cutting . 3
5.3 Mounting . 3
5.4 Grinding and polishing . 3
5.5 Etching . 3
6 Photomicrography . 4
6.1 General aspects . 4
6.2 Inspection . 4
6.3 Number of micrographs . 4
6.4 Optical microscopy . 4
6.5 Scanning electron microscopy . 5
7 Measurement of micrographs . 5
8 Calculation of results . 6
9 Interferences and uncertainties . 6
10 Test report . 7
Annex A (informative) Use of automatic image analysis (AIA). 9
Annex B (informative) Round-robin verification of this procedure .10
Annex C (informative) Results sheet — ISO 13383-2 .11
Bibliography .12
© ISO 2012 – All rights reserved iii

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kSIST FprEN ISO 13383-2:2015
ISO 13383-2:2012(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.
ISO 13383-2 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 13383-2:2015
INTERNATIONAL STANDARD ISO 13383-2:2012(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Microstructural characterization —
Part 2:
Determination of phase volume fraction by evaluation of
micrographs
1 Scope
This part of ISO 13383 specifies a manual method of making measurements for the determination of
the volume fraction of major phases in fine ceramics (advanced ceramics, advanced technical ceramics)
using micrographs of polished and etched sections, overlaying a square grid of lines, and counting the
number of intersections lying over each phase.
NOTE 1 This method assumes that the true phase volume fractions are equivalent to area fractions on a
randomly cut cross-section according to stereological principles.
NOTE 2 Guidelines for polishing and etching of advanced technical ceramics can be found in Annexes A and B
of ISO 13383-1:2012.
The method applies to ceramics with one or more distinct secondary phases, such as found in Al O /ZrO ,
2 3 2
Si/SiC, or Al O /SiC .
2 3 w
If the test material contains discrete pores, these are to be treated as a secondary phase for the purpose
of this method, provided that there is no evidence of grain pluck-out during polishing being confused
with genuine pores.
NOTE 3 If the material contains more than about 20 % porosity, there is a strong risk that the microstructure
will be damaged during the polishing process, and measurement of the volume fraction of pores may become
misleading. Secondary phase volume fractions or porosity present at levels of less than 0,05 are subject to
considerable error and potential scatter in results. A larger number of micrographs than the minimum of three is
normally needed to improve the consistency and accuracy of the results.
NOTE 4 Many ceramics contain small amounts of secondary glassy phases. In order to make a reasonable
estimate of glassy phase content, the glass material between crystalline grains should be readily observable, and
thus should be at least 0,5 µm in width. The method in this part of ISO 13383 is not considered appropriate for
narrow glassy films around grains.
NOTE 5 Microstructures are seldom homogeneous, and the phase contents can vary from micrograph to
micrograph. It is essential to survey a sufficiently wide area of the prepared section to ensure that those areas
selected for evaluation are representative, and do not contain eye-catching irregularities. This method assumes
that the selected regions of a prepared cross-section are statistically representative of the whole sampled section.
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 currently outside the scope of this
part, but some guidelines are given in Annex A.
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
© ISO 2012 – All rights reserved 1

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kSIST FprEN ISO 13383-2:2015
ISO 13383-2:2012(E)
3 Terms a nd definiti ons
For the purposes of this document, the following terms and definitions apply.
3.1
phase volume fraction
volume occupied by a distinct, identifiable phase present in a material expressed as a fraction of the whole
3.2
primary phase
principal phase within a microstructure, typically comprising more than 50 % by volume or observed
area in a cross-section
3.3
secondary phase
one or more distinct identifiable phases other than a primary crystalline phase in a material
NOTE A secondary phase can be in the form of discrete grains, or as a continuous phase surrounding some or all of
the major phase grains. For the purposes of this part of ISO 13383, porosity may be treated as a secondary phase.
4 Apparatus
4.1 Sectioning equipment
Any suitable method may be used for preparing the test section from the item under investigation. If a
diamond-bladed cut-off saw is employed, it is recommended that the grit size should not exceed 150 µm.
[5]
NOTE This grit size is designated as D151 according to ISO 6106 .
4.2 Mounting equipment
Suitable metallurgical mounting equipment and media for providing firm gripping of the test piece
for polishing.
4.3 Grinding and polishing equipment
Suitable grinding and polishing equipment, employing diamond abrasive media.
NOTE A sequence of abrasives and techniques recommended for polishing are given in Annex A of
ISO 13383-1:2012.
4.4 Microscope
An optical or scanning electron microscope with photomicrographic facilities.
NOTE Although the true magnification of the image is unimportant for making the measurement of the
volume fraction, it is advised that a reference graticule may be used to determine magnification in an optical
microscope, or a reference grid or latex spheres may be used for calibration of magnification in a scanning electron
microscope, and as a check on the homogeneity of magnification across the field of view.
An optical microscope is additionally required for assessing the quality of polishing (see 5.4).
4.5 Transparent grid
Transparent square grid on, e.g. acetate film, and with line thickness not exceeding 0,1 mm.
NOTE 1 The grid spacing selected is not critical, but may conveniently be between 3 mm and 15 mm to minimize
eyestrain. However, it is necessary that consideration of the requirements of 6.3 is taken into account.
2 © ISO 2012 – All rights reserved

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kSIST FprEN ISO 13383-2:2015
ISO 13383-2:2012(E)
NOTE 2 A suitable grid may be prepared as a computer plot with sufficient accuracy of line spacing for the
purposes of this part of ISO 13383.
5 Test piece preparation
5.1 Sampling
The test pieces shall be sampled in a manner subject to agreement between parties.
NOTE Guidance on this issue may be found in EN 1006 (see Bibliography [18]). Depending on the objectives
of performing the measurement, it is desirable to maintain knowledge of the positions within components or test
pieces from which sections are prepared.
5.2 Cutting
The required section of test piece shall be cut using the sectioning equipment (see 4.1).
NOTE For routine inspection of materials, a small area of side no more than 10 mm is normally adequate as
the section to be polished.
5.3 Mounting
Mount the test piece using an appropriate mounting medium.
NOTE 1 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 grinding and polishing.
NOTE 2 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 test pieces. The method of mounting selected should take into
account the etching procedure to be used; see Annex B.
5.4 Grinding and polishing
Grind and polish the surface of the test piece. Care shall 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 4.4) at high magnification. At least 90 % of the test piece area shall be
free from optically visible scratches, or other damage introduced by polishing, which will interfere with
the determination. In particular, avoid the plucking out of discrete secondary phases from the surface
giving the appearance of pores.
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 whil
...