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1、BRITISH STANDARD BS EN 623-3:2001 Advanced technical ceramics Monolithic ceramics General and textural properties Part 3: Determination of grain size and size distribution (characterized by the linear intercept method) The European Standard EN 623-3:2001 has the status of a British Standard ICS 81.0
2、60.30 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 623-3:2001 This British Standard, having been prepared under the direction of the Sector Committee for Materia
3、ls and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 August 2001 BSI 07-2001 ISBN 0 580 37672 9 National foreword This British Standard is the official English language version of EN 623-3:2001. It supersedes DD ENV 623-3:1993 which is withdrawn.
4、 The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implemen
5、t international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport
6、to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible European com
7、mittee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to
8、 22, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c)
9、BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 623-3 May 2001 ICS 81.060.30Supersedes ENV 623-3:1993 English version Advanced technical ceramics Monolithic ceramics General and textural properties Part 3: Determination of grain size and size distribution (characterized by the linear interc
10、ept method) Cramiques techniques avances Mthodes dessai pour cramiques monolithiques Proprits gnrales et texturales Partie 3: Dtermination de la taille des grains Hochleistungskeramik Monolithische Keramik Allgemeine und strukturelle Eigenschaften Teil 3: Bestimmung der Korngre This European Standar
11、d was approved by CEN on 19 April 2001. 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
12、 national standards may be obtained on application to the 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
13、 notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerlan
14、d and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 6
15、23-3:2001 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 2 EN 623-3:2001 BSI 07-2001 Contents Page Foreword . 3 1 Scope.3 2 Normative references 3 3 Terms and definitions4 4 Significance and use4 5 Apparatus.5 6 Test piece preparatio
16、n .6 7 Photomicrography.7 8 Measurement of micrographs8 9 Calculation of results.10 10 Interferences and uncertainties10 11 Test Report11 Annex A (informative) Bibliography on stereology and grain size measurement.13 Annex B (informative) Grinding and polishing procedures.14 Annex C (informative) Et
17、ching procedures .16 Annex D (informative) Setting Khler illumination in an optical microscope18 Annex E (informative) Round-robin verification of the procedure in this standard19 Annex F (informative) Grain size distribution measurement.21 Annex G (informative) Results sheet Grain size in accordanc
18、e with EN 623-3.22 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 623-3:2001 BSI 07-2001 Foreword This European Standard has been prepared by Technical Committee CEN/TC 184, Advanced technical ceramics, the Secretariat of which is
19、 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 November 2001, and conflicting national standards shall be withdrawn at the latest by November 2001. This European Standard supersedes
20、 ENV 623-3:1993. Annexes A, B, C, D, E, F and G are informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Gree
21、ce, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. 1Scope This part of EN 623 describes manual methods of making measurements for the determination of mean linear intercept grain size of advanced technical ceramics using photomi
22、crographs of polished and etched test pieces. This is not the true mean grain diameter, but a somewhat smaller parameter representing the average path length of a line drawn across a two-dimensional section. The relationship to true grain dimensions depends on grain shape and degree of microstructur
23、al anisotropy. This standard contains two methods: A and B. Method A applies to single-phase ceramics, and to ceramics with a principal crystalline phase and a glassy grain boundary phase of less than about 5 % by volume for which intercept counting suffices. Method B applies to ceramics with more t
24、han about 5 % by volume of pores or secondary phases, or ceramics with more than one major crystalline phase where individual intercept lengths are measured, which can optionally be used to create a size distribution. This latter method allows the pores or phases to be distinguished and the mean lin
25、ear intercept size for each to be calculated separately. NOTE A method of determining volume fraction(s) of secondary phase(s) is under development as ENV 623-5; this will provide a means of determining whether Method A or Method B should be applied in borderline cases. Some users of this standard m
26、ay wish to apply automatic or semiautomatic image analysis to micrographs or directly captured microstructural images. This is permitted by this standard provided that the technique employed simulates the manual method (see clause 4 and 8.4). 2Normative references This European Standard incorporates
27、, 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 S
28、tandard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 4 EN 623-3:2001 BSI
29、07-2001 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). 3Terms and definitions For the purposes
30、of this European Standard, the following terms and definitions apply. 3.1 grain size size of the distinct crystals in a material and, for the purposes of this method of test, that of the primary or major phase 3.2 mean linear intercept grain size the average value of the distance between grain bound
31、aries as shown by randomly positioned lines drawn across a micrograph or other image of the microstructure 4Significance and use The mean grain size and the distribution of grain sizes of a ceramic material play an important role in determining many properties, and thus grain size characterization i
32、s an important tool for ensuring consistency of manufacture. There are many measures of grain size and/or shape, but the linear intercept method provides the simplest possible method from a two-dimensional section through the material. However, it must be recognised that the numerical value obtained
33、 for the mean linear intercept size is somewhat smaller than most other measures of grain size because intercepts can cross grains at any position, and not necessarily along the largest axis. The relationship between mean linear intercept size and a true three-dimensional grain size is not simple, a
34、nd depends on the grain shape and the average number of facets. NOTE Annex A contains a bibliography of sources dealing with stereology and methods of sizing three-dimensional objects. This standard provides a simple method of measuring intercept distances in single-phase materials based on counting
35、 the number of intersections along given lengths of randomly orientated and positioned lines or randomly positioned circles drawn onto a micrograph of a suitably sectioned, polished and etched test piece. The length of lines crossing large pores residing at grain boundaries can be ignored, thus elim
36、inating any bias that porosity may introduce, but small pores within grains should be ignored. In materials which contain more than one phase, the phases may be continuous or as isolated grains. It may be necessary to characterize the different phases separately. The principal purpose of this standa
37、rd is to permit characterization of the major phases. The same intercept principle as for single-phase materials can be used, but the individual intercept lengths across each phase must be measured, rather than just counted. The characterization of minor phases may require different treatment, which
38、 is outside the scope of this standard. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 5 EN 623-3:2001 BSI 07-2001 If the material possesses a microstructure which has a preferred orientation of the primary or secondary phases, the res
39、ults of this measurement may not be representative of the true character of the material. Rather than using randomly orientated lines, it may be necessary to make measurements restricted to specific orientations. If undertaken, this must be reported in the report. This standard does not cover method
40、s of measuring mean grain size by counting using calibrated microscope stage movement or projection onto screens, accompanied by visual observation. While this latter method may produce an equivalent result to the analysis of micrographs, it does not provide a means of verification of the results of
41、 the measurement, since no permanent record is obtained. If automatic or semiautomatic image analysis (AIA) is to be used it must be recognised that different AIA systems approach the measurement in different ways, and may use different parameters to linear intercept distance, such as those based on
42、 grain area by pixel counting. In order to obtain results equivalent to those of the manual method described in this standard, the AIA system needs to be programmed to operate in a similar way to the manual method. By agreement between parties, such a near-equivalent AIA method may be used as an alt
43、ernative to the manual method, and if undertaken must be reported in the report. 5Apparatus 5.1Sectioning 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 mm to 150 mm and shall be cooled.
44、NOTE The grit size is designated D151 in ISO 6106, see annex A. 5.2Mounting equipment Suitable metallurgical mounting equipment and media for providing firm gripping of the test pieces for polishing. 5.3Grinding and polishing equipment Suitable grinding and polishing equipment, employing diamond abr
45、asive media. NOTE Annex B recommends techniques and abrasives. 5.4Microscope An optical or scanning electron microscope with photomicrographic facilities. A reference graticule is required for determination of magnification in an optical microscope, and a reference square grid or latex spheres are r
46、equired for calibration of magnification in a scanning electron microscope. In all cases, the calibration of dimensions of the references shall be traceable to national or international standards of length measurement. An optical microscope is additionally required for assessing quality of polishing
47、 (see 6.4). Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 13 15:58:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 6 EN 623-3:2001 BSI 07-2001 5.5Calibrated rule or scale A calibrated rule or scale reading to better than 0.5 mm and accurate to better than 0,5 %. 6Test piece preparation 6.1
48、Sampling The test pieces shall be sampled in accordance with the guidelines given in ENV 1006, and subject to agreement between parties. NOTE Depending on the objectives of the measurement, it is desirable to maintain full knowledge of the positions within components or test pieces from which sectio
49、ns are prepared. 6.2Cutting The required section of the test piece shall be cut using the diamond saw (see 5.1). NOTE For routine inspection of materials, a small area of not more than 10 mm side is normally adequate as the section to be polished. 6.3Mounting 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 vacuum impregnate the test piece with liquid mounting resin before encapsulating as thi