EN 623-5:2009

1 Scope
2 Normative references
3 Terms and definitions
4 Apparatus
   4.1 Sectioning equipment
   4.2 Mounting equipment
   4.3 Grinding and polishing equipment
   4.4 Microscope
   4.5 Transparent grid
5 Test piece preparation
   5.1 Sampling
   5.2 Cutting
   5.3 Mounting
   5.4 Grinding and polishing
   5.5 Etching
6 Photomicrography
   6.1 General aspects
   6.2 Inspection
   6.3 Number of micrographs
   6.4 Optical microscopy
   6.5 Scanning electron microscopy (SEM)
7 Measurement of micrographs
8 Calculation of results
9 Interferences and uncertainties
10 Test report
Annex A (informative) - Grinding and polishing
                        procedures
Annex B (informative) - Etching procedures
Annex C (informative) - Use of automatic image
                        analysis (AIA)
   C.1 Background
   C.2 Analysis techniques
   C.3 Micrograph requirements
   C.4 Calibration
Annex D (informative) - Setting Köhler illumination in
                        an optical microscope
   D.1 Purpose
   D.2 Definition
   D.3 Setting up for Köhler illumination
Annex E (informative) - Round robin verification of this
                        procedure
Annex F (informative) - Results sheet
Bibliography

This part of EN 623 specifies a manual method of making measurements for the determination of volume fraction ofmajor phases in advanced technical ceramics using micrographs of polished and etched sections, overlaying a squaregrid 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 crosssectionaccording 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,orAl2O3/SiCw.If the test material contains discrete pores, these can be treated as a secondary phase for the purpose of this methodprovided 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 damagedduring 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 andpotential scatter in results. A larger number of micrographs than the minimum of three is normally needed to improvethe consistency and accuracy of the results.NOTE 4 Many ceramics contain small amounts of secondary glassy phases. In order to make a reasonable estimate ofglassy phase content, the glass material between crystalline grains should be readily observable, and thus should be at least0,5 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 wholesampled section.