1、BS EN 623-5:2009ICS 81.060.30NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDAdvanced technicalceramics Monolithicceramics Generaland textural propertiesPart 5: Determination of phase volumefraction by evaluation of micrographsCopyright European Committee for St
2、andardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2009 BSI 2009ISBN 978 0 580 63844 2Amendments/cor
3、rigenda issued since publicationDate CommentsBS EN 623-5:2009National forewordThis British Standard is the UK implementation of EN 623-5:2009. It supersedes DD ENV 623-5:2002 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/13, Advanced technical cer
4、amics.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunityf
5、rom legal obligations.Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 623-5:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 623-5July 2009ICS 81.060.30 Supersedes ENV
6、 623-5:2002 English VersionAdvanced technical ceramics - Monolithic ceramics - Generaland textural properties - Part 5: Determination of phase volumefraction by evaluation of micrographsCramiques techniques avances - Cramiquesmonolithiques - Proprits gnrales et textures - Partie 5:Dtermination de la
7、 fraction volumique de phase parvaluation des microphotographiesHochleistungskeramik - Monolithische Keramik -Allgemeine und strukurelle Eigenschaften - Teil 5:Bestimmung des Volumenanteils von Phasen durchAuswertung von MikrogefgeaufnahmenThis European Standard was approved by CEN on 19 June 2009.C
8、EN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on appl
9、ication 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre ha
10、s the same status as theofficial 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, Portu
11、gal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reser
12、vedworldwide for CEN national Members.Ref. No. EN 623-5:2009: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 623-5:2009EN 623-5:2009 (E) 2 Contents page 1 Scope 42 Normat
13、ive references 43 Terms and definitions . 54 Apparatus . 54.1 Sectioning equipment . 54.2 Mounting equipment 54.3 Grinding and polishing equipment 54.4 Microscope . 54.5 Transparent grid 55 Test piece preparation 65.1 Sampling . 65.2 Cutting 65.3 Mounting . 65.4 Grinding and polishing . 65.5 Etching
14、 66 Photomicrography . 76.1 General aspects . 76.2 Inspection . 76.3 Number of micrographs 76.4 Optical microscopy 76.5 Scanning electron microscopy (SEM) . 77 Measurement of micrographs 88 Calculation of results 89 Interferences and uncertainties . 910 Test report 9Annex A (informative) Grinding an
15、d polishing procedures . 11Annex B (informative) Etching procedures . 13Annex C (informative) Use of automatic image analysis (AIA) 14C.1 Background 14C.2 Analysis techniques 14C.3 Micrograph requirements . 14C.4 Calibration 14Annex D (informative) Setting Khler illumination in an optical microscope
16、 15D.1 Purpose . 15D.2 Definition 15D.3 Setting up for Khler illumination 15Annex E (informative) Round robin verification of this procedure . 16Annex F (informative) Results sheet 17Bibliography 18Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleN
17、o reproduction or networking permitted without license from IHS-,-,-BS EN 623-5:2009EN 623-5:2009 (E) 3 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 g
18、iven 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 m
19、ay 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 textura
20、l 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 o
21、f 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
22、, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Copyright European Committee for Standardization Provided by IHS under license with CENNot
23、 for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 623-5:2009EN 623-5:2009 (E) 4 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 o
24、f 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. N
25、OTE 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
26、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 polish
27、ing 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 ne
28、eded 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
29、0,5 m 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 homogen
30、eous, 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
31、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
32、 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
33、 for the evaluation of properties EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted withou
34、t license from IHS-,-,-BS EN 623-5:2009EN 623-5:2009 (E) 5 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 whol
35、e 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 European Standard, poros
36、ity 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 m to 150 m and shall be cooled. NOTE This grit size is designated D151 a
37、ccording 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 ab
38、rasives 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 ref
39、erence 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
40、 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,
41、 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 European Standard. Copyright European Committee for Standardization Provided by IHS under
42、license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 623-5:2009EN 623-5:2009 (E) 6 5 Test piece preparation 5.1 Sampling The test pieces shall be sampled in accordance with the guidelines given in EN 1006, and subject to agreement between parties.
43、NOTE 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 diamond saw (see 4.1). NOTE For routine insp
44、ection 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. If the ceramic is suspected to have significant open porosity in some regions (see Clause 1) it is advisable to vac
45、uum impregnate the test piece with liquid mounting resin before encapsulating as this will provide some support during grinding and 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
46、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. Ca
47、re 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 4.4) at high magnificati
48、on. 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, discrete secondary phases may be plucked out from the surface giving the appearance of pores. This shall be avoided. NOTE Care should be taken in choosing the sequence of grits and lap types. It is impossible within the scope of this part of EN 623 to make specific recommendations for all types of material. The ge
