SIST ENV 623-5:2007

SLOVENSKI STANDARD
01-januar-2007
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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 strukturelle
Eigenschaften - Teil 5: Bestimmung des Volumenanteils von Phasen durch Auswertung
von Mikrogefügeaufnahmen
Céramiques techniques avancées - Méthodes d'essai pour céramiques monolithiques -
Propriétés générales et texturales
Ta slovenski standard je istoveten z: ENV 623-5:2002
ICS:
81.060.30 Sodobna keramika Advanced ceramics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN PRESTANDARD
ENV 623-5
PRÉNORME EUROPÉENNE
EUROPÄISCHE VORNORM
July 2002
ICS 81.060.30
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 - Méthodes d'essai pour Hochleistungskeramik - Monolithische Keramik -
céramiques monolithiques - Propriétés générales et Allgemeine und strukturelle Eigenschaften - Teil 5:
texturales Bestimmung des Volumenanteils von Phasen durch
Auswertung von Mikrogefügeaufnahmen
This European Prestandard (ENV) was approved by CEN on 12 March 2002 as a prospective standard for provisional application.
The period of validity of this ENV is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the ENV can be converted into a European Standard.
CEN members are required to announce the existence of this ENV in the same way as for an EN and to make the ENV available promptly
at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the ENV) until the final
decision about the possible conversion of the ENV into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. ENV 623-5:2002 E
worldwide for CEN national Members.

Contents
page
Foreword.3
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.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).15
Annex D (informative)  Setting Köhler illumination in an optical microscope.16
Annex E (informative)  Round robin verification of this procedure .17
Annex F (informative)  Results sheet .18
Bibliography .19
Foreword
This document ENV 623-5:2002 has been prepared by Technical Committee CEN/TC 184 "Advanced technical
ceramics", the secretariat of which is held by BSI.
Annexes A to F are all informative.
This Prestandard includes a Bibliography.
EN 623 consists of five Parts:
Part 1: Determination of the presence of the presence of defects by dye penetration tests
Part 2: Determination of density and porosity
Part 3: Determination of grain size
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 announce this European Prestandard: Austria, Belgium, Czech Republic, Denmark, Finland,
France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain,
Sweden, Switzerland and the United Kingdom.
1 Scope
This European Prestandard 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 Prestandard 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 containing eye-catching irregularities.
Some users of this Prestandard can wish to apply automatic or semiautomatic image analysis to micrographs or
directly captured microstructural images. This is currently outside the scope of this Prestandard, but some guidelines
are given in annex C.
2 Normative references
This European Prestandard incorporates by dated or undated reference provisions from other publications. These
normative references are cited at the appropriate places in the text and the publications are listed hereafter. For
dated references, subsequent amendments to or revisions of any of these publications apply to this European
Prestandard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
ENV 1006 Advanced technical ceramics - Methods of testing monolithic ceramics - Guidance on the sampling
and selection of test pieces
EN ISO/IEC 17025 General requirements for the competence of testing and calibration laboratories (ISO/IEC
17025:1999)
3 Terms and definitions
For the purposes of this European Prestandard, 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 secondary phase can be in the form of discrete grains, or as a continuous phase surrounding some or all the
major phase grains. For the purposes of this Prestandard, porosity may be treated as a secondary phase.
4 Apparatus
4.1 Sectioning equipment
A suitable diamond-bladed cut-off saw to prepare the initial section for investigation. The saw shall be metal bonded
with a diamond grit size of 125 μm to 150 μm and shall be cooled.
NOTE This grit size is designated D151 according to ISO 6106, see [1].
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.
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 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 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 minimise eyestrain.
However, it is necessary that consideration of the requirements of 6.3 is taken into account.
NOTE 2 A suitable grid may be prepared as a computer plot with sufficient accuracy of line spacing for the purposes of this
Prestandard.
5 Test piece preparation
5.1 Sampling
The test pieces shall
...