BS EN 623-5-2009 Advanced technical ceramics - Monolithic ceramics - General and textural properties - Part 5 Determination of phase volume nfraction by evaluation of micrographs《高.pdf

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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 micrographsLicensed Copy: Wang Bin, ISO/EXCHAN

2、GE CHINA STANDARDS, 01/12/2009 02:51, Uncontrolled Copy, (c) BSIThis 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/corrigenda issued since publicationDate CommentsBS EN 623-5:2009National f

3、orewordThis 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 It supersedes DD ENV 623-5:2002 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/13, Advanced technical ceramics.A list of organizations represented on this committee can be obta

4、ined 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 immunityfrom legal obligations.Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STAND

5、ARDS, 01/12/2009 02:51, Uncontrolled Copy, (c) BSIBS EN 623-5:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 623-5July 2009ICS 81.060.30 Supersedes ENV 623-5:2002 English VersionAdvanced technical ceramics - Monolithic ceramics - Generaland textural properties - Part 5: Determination of phase

6、 volumefraction by evaluation of micrographsCramiques techniques avances - Cramiquesmonolithiques - Proprits gnrales et textures - Partie 5:Dtermination de la fraction volumique de phase parvaluation des microphotographiesHochleistungskeramik - Monolithische Keramik -Allgemeine und strukurelle Eigen

7、schaften - Teil 5:Bestimmung des Volumenanteils von Phasen durchAuswertung von MikrogefgeaufnahmenThis 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 EuropeanStandard the s

8、tatus of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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).

9、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 has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic,

10、 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 STANDARDIZATIONCOMIT EUROPEN DE NORMALIS

11、ATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 623-5:2009: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/12/2009 02:51, Uncont

12、rolled Copy, (c) BSIBS EN 623-5:2009EN 623-5:2009 (E) 2 Contents page 1 Scope 42 Normative 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

13、65.1 Sampling . 65.2 Cutting 65.3 Mounting . 65.4 Grinding and polishing . 65.5 Etching 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

14、89 Interferences and uncertainties . 910 Test report 9Annex A (informative) Grinding and 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

15、Calibration 14Annex D (informative) Setting Khler illumination in an optical microscope 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 18Licensed Copy:

16、Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/12/2009 02:51, Uncontrolled Copy, (c) BSIBS 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 Sta

17、ndard 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

18、 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 - Gen

19、eral 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:

20、 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,

21、 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. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/12/2009 02:51, U

22、ncontrolled Copy, (c) BSIBS 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 of polished and etched sections, overlaying a square gri

23、d 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

24、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 pro

25、vided 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 pore

26、s 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 res

27、ults. 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 m in width. The method in this European Standard is

28、 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 t

29、o 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 anal

30、ysis 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 refere

31、nces, 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, Gen

32、eral requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/12/2009 02:51, Uncontrolled Copy, (c) BSIBS EN 623-5:2009EN 623-5:2009 (E) 5 3 Terms and definitions For the purposes of this part of EN 623, th

33、e 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 sec

34、ondary 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, porosity may be treated as a secondary phase. 4 Apparatus 4.1 Sectioning equipment A suitable diamond-bladed cut-off saw to prepare

35、 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 according to ISO 6106, see 1. 4.2 Mounting equipment Suitable metallurgical mounting equipment and media for providing firm gri

36、pping 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 microsco

37、pe 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

38、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,

39、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 a

40、s a computer plot with sufficient accuracy of line spacing for the purposes of this European Standard. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/12/2009 02:51, Uncontrolled Copy, (c) BSIBS EN 623-5:2009EN 623-5:2009 (E) 6 5 Test piece preparation 5.1 Sampling The test pieces shall be

41、 sampled in accordance with the guidelines given in EN 1006, and subject to agreement between parties. 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

42、 The required section of test-piece shall be cut using the diamond saw (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. If the ceram

43、ic 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 It is not essential to encapsulate the test piece

44、. 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

45、 to be used; see Annex B. 5.4 Grinding and polishing Grind and polish the surface of the test piece. Care 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 unti

46、l 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, discret

47、e 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

48、. The general principle to be adopted is the minimisation of subsurface damage, and its removal by progressively finer grits whilst retaining a flat surface. Some guidelines on polishing are given in Annex A. 5.5 Etching When a good quality polished surface has been achieved, the test piece shall be

49、 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. NOTE 2 For optical evaluation, it is usually necessary to etch oxide materials in such a way that the individual phases are distinguis