DIN EN 1071-10-2009 Advanced technical ceramics - Methods of test for ceramic coatings - Part 10 Determination of coating thickness by cross sectioning English version of DIN EN 10.pdf

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1、October 2009DEUTSCHE NORM English price group 10No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 81.060.30!$Z?L“1552841

2、www.din.deDDIN EN 1071-10Advanced technical ceramics Methods of test for ceramic coatings Part 10: Determination of coating thickness by cross sectioningEnglish version of DIN EN 1071-10:2009-10Hochleistungskeramik Verfahren zur Prfung keramischer Schichten Teil 10: Bestimmung der Schichtdicke mitte

3、ls QuerschliffEnglische Fassung DIN EN 1071-10:2009-10SupersedesDIN CEN/TS 1071-10:2004-10www.beuth.deDocument comprises pages17DIN EN 1071-10:2009-10 National foreword This standard has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, Working Group WG 5 “Ceramic coatin

4、gs” (Secretariat: BSI, United Kingdom). At present a DIN committee does not exist for this standard since the parties concerned have not shown any interest in work on the subject. The Normenausschuss Materialprfung (Materials Testing Standards Committee) is obliged to publish the standard, however,

5、as the subject falls in its domain. Amendments This standard differs from DIN CEN/TS 1071-10:2004-10 as follows: a) The standard has been editorially revised. Previous editions DIN CEN/TS 1071-10: 2004-10 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1071-10 July 2009 ICS 81.060.30 Supersed

6、es CEN/TS 1071-10:2004 English Version Advanced technical ceramics Methods of test for ceramic coatings Part 10: Determination of coating thickness by cross sectioningCramiques techniques avances Mthodes dessai pour les revtements cramiques Partie 10: Dtermination de lpaisseur du revtement par dcoup

7、age transverse Hochleistungskeramik Verfahren zur Prfung keramischer Schichten Teil 10: Bestimmung der Schichtdicke mittels Querschliff This 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

8、 for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three off

9、icial 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 has the same status as theofficial versions. CEN members are the national standards bodies of Austria,

10、 Belgium, Bulgaria, Cyprus, Czech Republic, 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

11、 FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1071-10:2009: E2 Contents Page Foreword .

12、3 Introduction 5 1 Scope 6 2 Normative 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 Spec

13、imen tilt 7 6.5 Coating damage 7 6.6 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 Uniform

14、ity of magnification . 9 7.8 Stability 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)

15、 General guidance on the preparation 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 EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 3 Foreword This document (EN 1071

16、-10:2009) 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 given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by January 2010,

17、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 may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. T

18、his document supersedes CEN/TS 1071-10:2004. 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 Par

19、t 3: Determination of adhesion and other mechanical 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 t

20、est Part 7: Determination of hardness and 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 inter

21、nal stress by the Stoney formula Part 12: 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 t

22、his European Standard. EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 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,

23、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. EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 5 Introduction The thickness of

24、a coating is an important property that controls its 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 descr

25、ibed here is direct, but is destructive, requiring preparation 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). EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 6 1 Scope This document specifie

26、s a method of measuring the thickness of ceramic coatings 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 co

27、atings and current best practice. 2 Normative references 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) app

28、lies. ENV 13005, Guide to the expression of uncertainty in 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

29、thickness mean of the thickness measurements, of which a 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

30、 cross-section requires care to ensure that the total thickness 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

31、 directly using a modern measuring microscope, or indirectly 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 commercial

32、ly. 5.2 Optical microscope The optical microscope shall have 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

33、, can be used directly to measure coating thickness without the need EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 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

34、the coating to be measured and the accuracy required. 6 Sample 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 magnifica

35、tion to be used for measurement; c) all material damaged by cutting 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 roug

36、hness If the coating or its substrate is rough relative to the 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

37、perpendicular to the plane of the coating, the measured thickness 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 prepare

38、d using the same procedures as the test sample as a check on the 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 compo

39、unded if the test specimen tilt is different from that used during 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

40、 rounded, i.e. if the coating cross-section is not completely 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). EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 8 6.7 Over

41、plating Overplating of the test specimen serves to protect the coating 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 Op

42、timum etching will produce a clearly defined and narrow line at the 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 Smeari

43、ng Polishing may leave smeared metal that obscures the true boundary 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 significan

44、t variation in readings is an indication of possible smearing. 7 Calibration 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 shou

45、ld be checked with a graticule over the area to be used in the measurement. 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

46、 of clause 9. The stability of the calibration shall be checked at 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 Measure

47、ment 7.3.1 Measure the perpendicular edge-to-edge distance between 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 dete

48、rmine the average spacing. 7.4 Calculation of magnification Calculate the magnification of the photograph by dividing the average of the measurements between selected lines by the certified distance between the lines: EN 1071-10:2009 (E) DIN EN 1071-10:2009-10 9 1000=cmlly (1) where y is the magnifi

49、cation; lmis the average of the measured distance, in millimetres, on the 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 contrast. 7.6 Magnification For a given coating thickness, measurement errors tend to increase with decreasing magnification. If practicable, th