EN 623-5:2009
(Main)Advanced technical ceramics - Monolithic ceramics - General and textural properties - Part 5: Determination of phase volume fraction by evaluation of micrographs
Advanced technical ceramics - Monolithic ceramics - General and textural properties - Part 5: Determination of phase volume fraction by evaluation of micrographs
This part of EN 623 specifies a manual method of making measurements for the determination of volume fraction of
major phases in 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 crosssection
according to stereological principles.
NOTE 2 Guidelines for polishing and etching of advanced technical ceramics can be found in Annexes A and B.
The method applies to ceramics with one or more distinct secondary phases, such as found in Al2O3/ZrO2, Si/SiC,or
Al2O3/SiCw.
If the test material contains discrete pores, these can 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 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 European Standard is not considered appropriate for narrow glassy films around grains.
This method assumes that the selected regions of a prepared cross-section are statistically representative of the whole
sampled section.
Hochleistungskeramik - Monolithische Keramik - Allgemeine und strukurelle Eigenschaften - Teil 5: Bestimmung des Volumenanteils von Phasen durch Auswertung von Mikrogefügeaufnahmen
Dieser Teil von EN 623 legt ein manuelles Messverfahren zur Bestimmung des Volumenanteils der Haupt-phasen in Hochleistungskeramiken fest, indem auf Mikrogefügeaufnahmen polierter und geätzter Quer-schnitte ein quadratisches Liniengitter aufgelegt und die Anzahl der Schnittpunkte der Gitterlinien über jeder Phase ausgezählt werden. 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 in den Anhängen A und B nachgelesen werden. Das Verfahren gilt für keramische Werkstoffe mit einer oder mehreren deutlich erkennbaren Sekundär-phase(n), die z. B. in Al2O3/ZrO2, Si/SiC oder in Al2O3/SiCw gefunden werden. Falls der zu untersuchende Werkstoff diskrete Poren enthält, können sie im Rahmen dieses Verfahrens als Sekundärphase angesehen werden, sofern es keine Hinweise darauf gibt, dass beim Polieren Körner aus dem Gefüge herausgebrochen wurden, die mit echten Poren verwechselt werden könnten. ANMERKUNG 3 Falls der Werkstoff eine Porosität von mehr als etwa 20 % aufweist, ist das Risiko groß, dass beim Polieren eine Schädigung des Feingefüges aufgetreten ist und ein irreführender Porenvolumenanteil ermittelt werden 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. Üblicherweise müssen, um Konsistenz und Genauigkeit der Ergebnisse zu verbessern, mehr als die Mindest-anzahl von drei Mikrogefügeaufnahmen ausgewertet werden. ANMERKUNG 4 Viele Keramiken enthalten kleine Mengen glasartiger Sekundärphasen.
Céramiques techniques avancées - Céramiques monolithiques - Propriétés générales et textures - Partie 5: Détermination de la fraction volumique de phase par évaluation des microphotographies
La présente partie de l'EN 623 spécifie une méthode manuelle de mesurage permettant de déterminer la
fraction volumique des principales phases dans les céramiques techniques avancées à l'aide de
microphotographies de parties polies et décapées, en recouvrant une grille carrée de lignes, et en comptant le
nombre d'intersections se trouvant sur chaque phase.
NOTE 1 Cette méthode suppose que les fractions volumiques de phase véritables sont équivalentes aux fractions de
surface sur une section transversale coupée de façon aléatoire selon les principes stéréologiques.
NOTE 2 Les directives de polissage et de décapage des céramiques techniques avancées sont mentionnées
en Annexes A et B.
La méthode s'applique aux céramiques avec une ou plusieurs phases secondaires distinctes, telles que dans
Al2O3/ZrO2, Si/SiC, ou dans Al2O3/SiCw.
Si le matériau d'essai contient des pores discrets, ceux-ci peuvent être traités en tant que phase secondaire
pour les besoins de la présente méthode sous réserve qu'il n'y ait pas de preuve d'arrachage de grain au
cours du polissage pouvant être confondu avec les pores réels.
NOTE 3 Si le matériau contient plus de 20 % de porosité environ il existe un risque majeur d'endommagement de la
microstructure au cours du processus de polissage, et le mesurage de fraction volumique des pores peut être faussé.
Les fractions volumiques de phase secondaire ou la porosité, présentes à des niveaux inférieurs à 0,05
constituent une source d'erreur considérable et de dispersion potentielle des résultats. Un nombre de
microphotographies supérieur au nombre minimum de trois microphotographies est normalement requis afin
d'améliorer l'uniformité et la précision des résultats.
Sodobna tehnična keramika - Monolitna keramika - Splošne in strukturne lastnosti - 5. del: Določanje volumenskega deleža faz z vrednotenjem mikrostrukture
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-november-2009
1DGRPHãþD
SIST ENV 623-5:2007
6RGREQDWHKQLþQDNHUDPLND0RQROLWQDNHUDPLND6SORãQHLQVWUXNWXUQHODVWQRVWL
GHO 'RORþDQMHYROXPHQVNHJDGHOHåDID]]YUHGQRWHQMHPPLNURVWUXNWXUH
Advanced technical ceramics - Monolithic ceramics - General and textural properties -
Part 5: Determination of phase volume fraction by evaluation of micrographs
Hochleistungskeramik - Monolithische Keramik - Allgemeine und strukurelle
Eigenschaften - Teil 5: Bestimmung des Volumenanteils von Phasen durch Auswertung
von Mikrogefügeaufnahmen
Céramiques techniques avancées - Céramiques monolithiques - Propriétés générales et
textures - Partie 5: Détermination de la fraction volumique de phase par évaluation des
microphotographies
Ta slovenski standard je istoveten z: EN 623-5:2009
ICS:
81.060.30 Sodobna keramika Advanced ceramics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD
EN 623-5
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2009
ICS 81.060.30 Supersedes ENV 623-5:2002
English Version
Advanced technical ceramics - Monolithic ceramics - General
and textural properties - Part 5: Determination of phase volume
fraction by evaluation of micrographs
Céramiques techniques avancées - Céramiques Hochleistungskeramik - Monolithische Keramik -
monolithiques - Propriétés générales et textures - Partie 5: Allgemeine und strukurelle Eigenschaften - Teil 5:
Détermination de la fraction volumique de phase par Bestimmung des Volumenanteils von Phasen durch
évaluation des microphotographies Auswertung von Mikrogefügeaufnahmen
This European Standard was approved by CEN on 19 June 2009.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 623-5:2009: E
worldwide for CEN national Members.
Contents
page
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 5
4 Apparatus . 5
4.1 Sectioning equipment . 5
4.2 Mounting equipment. 5
4.3 Grinding and polishing equipment . 5
4.4 Microscope . 5
4.5 Transparent grid . 5
5 Test piece preparation . 6
5.1 Sampling . 6
5.2 Cutting . 6
5.3 Mounting . 6
5.4 Grinding and polishing . 6
5.5 Etching . 6
6 Photomicrography . 7
6.1 General aspects . 7
6.2 Inspection . 7
6.3 Number of micrographs . 7
6.4 Optical microscopy. 7
6.5 Scanning electron microscopy (SEM) . 7
7 Measurement of micrographs . 8
8 Calculation of results . 8
9 Interferences and uncertainties . 9
10 Test report . 9
Annex A (informative) Grinding and polishing procedures . 11
Annex B (informative) Etching procedures . 13
Annex C (informative) Use of automatic image analysis (AIA) . 14
C.1 Background . 14
C.2 Analysis techniques . 14
C.3 Micrograph requirements . 14
C.4 Calibration . 14
Annex D (informative) Setting Köhler illumination in an optical microscope . 15
D.1 Purpose . 15
D.2 Definition . 15
D.3 Setting up for Köhler illumination . 15
Annex E (informative) Round robin verification of this procedure . 16
Annex F (informative) Results sheet . 17
Bibliography . 18
Foreword
This document (EN 623-5:2009) has been prepared by Technical Committee CEN/TC 184 “Advanced technical
ceramics”, the secretariat of which is held by BSI.
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 January 2010, and conflicting national standards shall be withdrawn at the latest
by January 2010.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights.
CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes ENV 623-5:2002.
EN 623 consists of five parts, under the general title "Advanced technical ceramics - Monolithic ceramics - General and
textural properties":
Part 1: Determination of the presence of defects by dye penetration
Part 2: Determination of density and porosity
Part 3: Determination of grain size and size distribution (characterized by the Linear Intercept Method)
Part 4: Determination of surface roughness
Part 5: Determination of phase volume fraction by evaluation of micrographs
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, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,
Switzerland and the United Kingdom.
1 Scope
This part of EN 623 specifies a manual method of making measurements for the determination of volume fraction of
major phases in 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.
The method applies to ceramics with one or more distinct secondary phases, such as found in Al O /ZrO , Si/SiC,or
2 3 2
Al O /SiC .
2 3 w
If the test material contains discrete pores, these can 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 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 European Standard is not considered appropriate for narrow glassy films around grains.
This method assumes that the selected regions of a prepared cross-section are statistically representative of the whole
sampled section.
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.
Some users of this European Standard can wish to apply automatic or semiautomatic image analysis to micrographs or
directly captured microstructural images. This is currently outside the scope of this European Standard, but some
guidelines are given in Annex C.
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.
EN 1006, Advanced technical ceramics - Monolithic ceramics - Guidance on the selection of test pieces for the
evaluation of properties
EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC
17025:2005)
3 Terms and definitions
For the purposes of this part of EN 623, 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
secondary phase
one or more distinct identifiable phases other than a primary crystalline phase in a material
NOTE A s
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.