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1、 W - - - - - - - - - - 7- - 7- 7- - - 6- 7- 7 7- 6 7 - - $ - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - W W D - w - - - - EN 1071-10:2009 (E) 2 Contents Page Foreword . 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Terms and definitions . 6 4 Principle . 6 5 Ap
2、paratus 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 Rounding of edges of the coating . 7 6.7 Overplating 8 6.8 Etchin
3、g . 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 Stability of magnification . 9 8 Test procedure 9 8.1 General . 9 8.2 Pre
4、paration 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 and measurement of cross- sections 13 A.1 Introduction . 13 A.2 C
5、utting 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) 3 Foreword This document (EN 1071-10:2009) has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, the secretariat of which is hel
6、d 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of an identical text or by endorsement, at the latest by January 2010, and conflicting national standards shall be withdrawn at the latest by January 2010. Attention is drawn to the possibility t
7、hat 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 1071-10:2004. EN 1071 Advanced technical ceramics Methods of test for ceramic coatings consis
8、ts 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 mechanical failure modes by a scratch test Part 4: Determination of chemical compos
9、ition 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 Youngs modulus by instrumented indentation testing withdrawn Part 8: Rockwell inde
10、ntation 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: Reciprocating wear test 1) Part 13: Determination of wear rate by the pin-on-disk
11、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. EN 1071-10:2009 (E) 4 According to the CEN/CENELEC Internal Regulations, the national standards org
12、anizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
13、Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. EN 1071-10:2009 (E) 5 Introduction The thickness of 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 coatin
14、gs. 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 preparation of a metallographic cross- section. A number of other standard non-destructive methods exist and some of
15、these are listed in the Bibliography (references 1 to 7). EN 1071-10:2009 (E) 6 1 Scope This document specifies 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 m
16、icroscope. 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 The following referenced document is indispensable for the application of this document. For dated references, only the edition cited
17、 applies. For undated references, the latest edition of the referenced document (including any amendments) applies. 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)
18、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 specified number is made within a reference area EN ISO 2064:2000 5 4 Principle This test procedure covers the measurement of coating
19、 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 thickness is revealed and that when viewed it is normal to the axis of the microscope. After proper calibration of the microscope, it is
20、 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 indirectly from photographic images obtained from an optical or scanning electron microscope. 5 Apparatus 5.1 Scanning electron microscope (
21、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 have a spatial resolution of 500 nm or better. Suitable instruments are available commercially. NOTE 1 Microscopes that incorporate a
22、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 without the need EN 1071-10:2009 (E) 7 to take photographs. This method is particularly useful where coating thickness variations around a
23、 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 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 fla
24、t 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 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
25、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 coating thickness, one or both of the interfaces bounding the coating may be too irregular to permit accurate measurement of the average thickness in
26、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 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
27、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 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 elec
28、tron beam or optical axis will result in an inaccurate measurement. This error is compounded 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-se
29、ction. 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 flat up to its edges, the observed thickness may differ from the true thickness. Edge rounding can be caused by improper mounting, grinding, polishing
30、or etching (see 6.8 and Annex A). EN 1071-10:2009 (E) 8 6.7 Overplating 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
31、 be exercised in the choice of plating procedure. 6.8 Etching Optimum 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 microsc
32、opy and do not necessarily enhance contrast in a SEM. 6.9 Smearing 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
33、polishing, etching and measurement several times. Any significant 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 tes
34、t specimen. For the case of stage movement calibration this should 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 th
35、e procedures specified in clause 8 and to the uncertainty limits 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 w
36、ith sufficient image contrast for later measurement. 7.3 Measurement 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 d
37、ifferent locations at least 3 mm apart on the photograph to determine 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
38、) 9 1000 c m l l y (1) where y is the magnification; lm is the average of the measured distance, in millimetres, on the image photograph; lc is 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 microscop
39、e 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, the magnification should be chosen so that th
40、e 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 Beca
41、use the magnification in an SEM may not be uniform over the entire field of view, errors can occur if both the calibration and measurement are not made over the same portion of the field. These errors can be significant. 7.8 Stability of magnification When using a SEM the magnification may drift wit
42、h time. This effect is minimised by mounting the stage micrometer or graticule along side the test specimen to keep the transfer time short. A change in the magnification can occur when adjustments are made with the focusing. 8 Test procedure 8.1 General Each instrument shall be operated (see clause
43、 7) in accordance with the manufacturers instructions. Appropriate attention shall be given to the factors listed in 7.5 to 7.8 and to the uncertainty requirements of clause 9. EN 1071-10:2009 (E) 10 8.2 Preparation of images 8.2.1 General Make a micrograph or record an image digitally of the test specimen under the same conditions and instrument settings as used for the calibration and make an appropriate measurement of t