1、BS EN1071-10:2009ICS 81.060.30NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDAdvanced technicalceramics Methodsof test for ceramiccoatingsPart 10: Determination of coatingthickness by cross sectioningThis British Standardwas published under theauthority of the
2、StandardsPolicy and StrategyCommittee on 31 August2009 BSI 2009ISBN 978 0 580 63849 7Amendments/corrigenda issued since publicationDate CommentsBS EN 1071-10:2009National forewordThis British Standard is the UK implementation of EN 1071-10:2009. Itsupersedes DD CEN/TS 1071-10:2004 which is withdrawn
3、.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 obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Us
4、ers are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS EN 1071-10:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 1071-10July 2009ICS 81.060.30 Supersedes CEN/TS 1071-10:2004 English VersionAdvanced technical ceramics
5、- Methods of test for ceramiccoatings - Part 10: Determination of coating thickness by crosssectioningCramiques techniques avances - Mthodes dessai pourles revtements cramiques - Partie 10: Dtermination delpaisseur du revtement par dcoupage transverseHochleistungskeramik - Verfahren zur Prfung keram
6、ischerSchichten - Teil 10: Bestimmung der Schichtdicke mittelsQuerschliffThis 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 status of a national stand
7、ard 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). A version in any other la
8、nguage 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, Denmark, Estonia, Finlan
9、d,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 NORMALISATIONEUROPISCHES KOMITEE
10、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 1071-10:2009: EBS EN 1071-10:2009EN 1071-10:2009 (E) 2 Contents Page Foreword . 3 Introduction 5 1 Scope 6 2 Normativ
11、e references . 6 3 Terms and definitions . 6 4 Principle . 6 5 Apparatus 6 5.1 Scanning electron microscope (SEM) 6 5.2 Optical microscope . 6 6 Sample preparation . 7 6.1 Cross-section preparation . 7 6.2 Surface roughness 7 6.3 Taper of cross-section 7 6.4 Specimen tilt 7 6.5 Coating damage 7 6.6
12、Rounding of edges of the coating . 7 6.7 Overplating 8 6.8 Etching . 8 6.9 Smearing 8 7 Calibration of instruments . 8 7.1 Procedure 8 7.2 Photography 8 7.3 Measurement . 8 7.4 Calculation of magnification 8 7.5 Poor contrast . 9 7.6 Magnification . 9 7.7 Uniformity of magnification . 9 7.8 Stabilit
13、y of magnification . 9 8 Test procedure 9 8.1 General . 9 8.2 Preparation of images 10 8.3 Measurement . 10 8.4 Thickness calculation . 10 8.5 Correction procedures . 11 9 Measurement uncertainty 11 10 Expression of results 11 11 Report . 11 Annex A (informative) General guidance on the preparation
14、and measurement of cross-sections 13 A.1 Introduction . 13 A.2 Cutting 13 A.3 Mounting 13 A.4 Grinding and polishing . 14 A.5 Use of the scanning electron microscope 14 Bibliography . 15 BS EN 1071-10:2009EN 1071-10:2009 (E) 3 Foreword This document (EN 1071-10:2009) has been prepared by Technical C
15、ommittee CEN/TC 184 “Advanced technical ceramics”, the secretariat of which is 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 January 2010, and conflicting national standards shall b
16、e withdrawn at the latest by January 2010. Attention is drawn to the possibility that some of the elements of 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 CEN/TS 1071-10:200
17、4. EN 1071 Advanced technical ceramics Methods of test for ceramic coatings consists of the following parts: Part 1: Determination of coating thickness by contact probe profilometer Part 2: Determination of coating thickness by the crater grinding method Part 3: Determination of adhesion and other m
18、echanical failure modes by a scratch test Part 4: Determination of chemical composition by electron probe microanalysis (EPMA) Part 5: Determination of porosity withdrawn Part 6: Determination of the abrasion resistance of coatings by a micro-abrasion wear test Part 7: Determination of hardness and
19、Youngs modulus by instrumented indentation testing withdrawn Part 8: Rockwell indentation test for evaluation of adhesion Part 9: Determination of fracture strain Part 10: Determination of coating thickness by cross sectioning Part 11: Determination of internal stress by the Stoney formula Part 12:
20、Reciprocating wear test 1) Part 13: Determination of wear rate by the pin-on-disk method 1)Parts 7, 8 and 11 are Technical Specifications. Part 7 was withdrawn shortly after publication of EN ISO 14577-4:2007. 1)In preparation at the time of publication of this European Standard. BS EN 1071-10:2009E
21、N 1071-10:2009 (E) 4 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, Germany, Greece, Hungary, Icel
22、and, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 1071-10:2009EN 1071-10:2009 (E) 5 Introduction The thickness of a coating is an important property that controls its
23、 functional behaviour. Thickness determinations are also used as part of quality control in the production of coatings. It is normal to specify a thickness when defining a coating, so that valid methods of measurement are required. The method described here is direct, but is destructive, requiring p
24、reparation of a metallographic cross-section. A number of other standard non-destructive methods exist and some of these are listed in the Bibliography (references 1 to 7). BS EN 1071-10:2009EN 1071-10:2009 (E) 6 1 Scope This document specifies a method of measuring the thickness of ceramic coatings
25、 by means of examination of a metallographically prepared cross-section of the coating in a calibrated optical or scanning electron microscope. It draws strongly on EN ISO 9220 8, modifying and updating as required to be relevant to ceramic coatings and current best practice. 2 Normative references
26、The following referenced document is indispensable 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. ENV 13005, Guide to the expression of uncertainty i
27、n measurement EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 3 Terms and definitions For the purposes of this document, the following term and definition apply. 3.1 local thickness mean of the thickness measurements, of which a
28、specified number is made within a reference area EN ISO 2064:2000 5 4 Principle This test procedure covers the measurement of coating thickness by examination of a cross-section in an optical or scanning electron microscope. Preparation of the cross-section requires care to ensure that the total thi
29、ckness is revealed and that when viewed it is normal to the axis of the microscope. After proper calibration of the microscope, it is a simple matter to determine the coating thickness from knowledge of the magnification used. This can be done directly using a modern measuring microscope, or indirec
30、tly from photographic images obtained from an optical or scanning electron microscope. 5 Apparatus 5.1 Scanning electron microscope (SEM) The SEM shall have a spatial resolution of 50 nm or better. Suitable instruments are available commercially. 5.2 Optical microscope The optical microscope shall h
31、ave a spatial resolution of 500 nm or better. Suitable instruments are available commercially. NOTE 1 Microscopes that incorporate a system to automatically record the XY coordinates are available and, if the stage movement has been calibrated, can be used directly to measure coating thickness witho
32、ut the need BS EN 1071-10:2009EN 1071-10:2009 (E) 7 to take photographs. This method is particularly useful where coating thickness variations around a component are likely. NOTE 2 The choice of instrument will depend on the thickness of the coating to be measured and the accuracy required. 6 Sample
33、 preparation 6.1 Cross-section preparation Prepare the cross-section so that: a) it is perpendicular to the plane of the coating; b) the surface is flat and the entire width of the coating image is simultaneously in focus at the magnification to be used for measurement; c) all material damaged by cu
34、tting or cross-sectioning is removed; d) the boundaries of the coating cross-section are sharply defined by no more than contrasting appearance, or by a narrow well defined line. NOTE Further guidance is given in Annex A. 6.2 Surface roughness If the coating or its substrate is rough relative to the
35、 coating thickness, one or both of the interfaces bounding the coating may be too irregular to permit accurate measurement of the average thickness in the field of view. 6.3 Taper of cross-section If the plane of the cross-section is not perpendicular to the plane of the coating, the measured thickn
36、ess will be greater than the true thickness. For example, an inclination of 10 degrees to the perpendicular will contribute an error of 1,5 %. NOTE It is recommended that a cross-section of a reference sample of known thickness be prepared using the same procedures as the test sample as a check on t
37、he accuracy of cutting, mounting and polishing procedures. 6.4 Specimen tilt Any tilt of the specimen (plane of cross-section) with respect to the electron beam or optical axis will result in an inaccurate measurement. This error is compounded if the test specimen tilt is different from that used du
38、ring calibration. 6.5 Coating damage Ceramic coatings are generally brittle, and hence easily damaged during preparation of the metallographic cross-section. 6.6 Rounding of edges of the coating If the edge of the coating cross-section is rounded, i.e. if the coating cross-section is not completely
39、flat up to its edges, the observed thickness may differ from the true thickness. Edge rounding can be caused by improper mounting, grinding, polishing or etching (see 6.8 and Annex A). BS EN 1071-10:2009EN 1071-10:2009 (E) 8 6.7 Overplating Overplating of the test specimen serves to protect the coat
40、ing during preparation of the cross-section and thus to prevent an inaccurate measurement. Removal of coating material is however possible during plating and care should be exercised in the choice of plating procedure. 6.8 Etching Optimum etching will produce a clearly defined and narrow line at the
41、 interface between the coating and substrate. A wide or poorly defined line can result in an inaccurate measurement. NOTE Many etchants are developed for optical microscopy and do not necessarily enhance contrast in a SEM. 6.9 Smearing Polishing may leave smeared metal that obscures the true boundar
42、y between the coating and the substrate, and/or the overplate and thus results in an inaccurate measurement. To help identify whether or not smearing occurs, repeat the polishing, etching and measurement several times. Any significant variation in readings is an indication of possible smearing. 7 Ca
43、libration of instruments 7.1 Procedure Each instrument shall be calibrated with a stage micrometer or graticule using an image taken under the same conditions as the test specimen. For the case of stage movement calibration this should be checked with a graticule over the area to be used in the meas
44、urement. When using an SEM, reference could also be made to ISO 16700 9. Appropriate attention shall be given to the factors listed below in subclauses 7.5 to 7.8, to the procedures specified in clause 8 and to the uncertainty limits of clause 9. The stability of the calibration shall be checked at
45、frequent intervals. 7.2 Photography Photograph the image of the micrometer scale or graticule. In the case of the SEM use a minimum signal-to-noise ratio of 2 to 1 and with sufficient image contrast for later measurement. 7.3 Measurement 7.3.1 Measure the perpendicular edge-to-edge distance between
46、the lines in the photographed image to the nearest 0,1 mm. Use a diffraction plate reader or equivalent for this measurement. 7.3.2 Repeat the measurement at least ten different locations at least 3 mm apart on the photograph to determine the average spacing. 7.4 Calculation of magnification Calcula
47、te the magnification of the photograph by dividing the average of the measurements between selected lines by the certified distance between the lines: BS EN 1071-10:2009EN 1071-10:2009 (E) 9 1000=cmlly (1) where y is the magnification; lmis the average of the measured distance, in millimetres, on th
48、e image photograph; lcis the certified distance, in micrometres. 7.5 Poor contrast The visual contrast between the substrate and the coating can be poor in both an optical microscope and a SEM. Etching for optical microscopy or, in the case of an SEM, use of the backscattered mode can improve contra
49、st. 7.6 Magnification For a given coating thickness, measurement errors tend to increase with decreasing magnification. If practicable, the magnification should be chosen so that the field of view is about 1,5 times the coating thickness. The magnification readout of an SEM often differs from the true magnification by more than the 5 % often quoted and, for some instruments, the magnification has been found to vary by 25 % across the field. 7.7 Uniformity of magnification Because the magnification in an SEM may not be un
