1、DRAFT FOR DEVELOPMENTDD CEN/TS 1071-11:2005Advanced technical ceramics Methods of test for ceramic coatings Part 11: Determination of internal stress by the Stoney formulaICS 81.060.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g
2、3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSIDD CEN/TS 1071-11:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Commi
3、ttee on 31 January 2007 BSI 2007ISBN 978-0-580-49935-7National forewordThis Draft for Development was published by BSI. It is the UK implementation of CEN/TS 1071-11:2005.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publicatio
4、ns and is of a provisional nature. It should be applied on this provisional basis, so that information and experience of its practical application can be obtained.Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organizat
5、ion responsible for its conversion to a European standard. A review of this publication will be initiated not later than 3 years after its publication by the European organization so that a decision can be taken on its status. Notification of the start of the review period will be made in an announc
6、ement in the appropriate issue of Update Standards.According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments sh
7、ould be sent to the Secretary of the responsible BSI Technical Committee at British Standards House, 389 Chiswick High Road, London W4 4AL.The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics.A list of organizations represented on RPI/13 ca
8、n be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Amendments issued since publicationAmd. No. Date CommentsLicensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 200
9、7, Uncontrolled Copy, (c) BSITECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 1071-11October 2005ICS 81.060.30English VersionAdvanced technical ceramics - Methods of test for ceramiccoatings - Part 11: Determination of internal stress by theStoney formulaCramiques techniqu
10、es avances - Mthodes dessaispour revtements cramiques - Partie 11 :Dtermination dela contrainte interne par la formule de StoneyHochleistungskeramik - Verfahren zur Prfung keramischerSchichten - Teil 11: Bestimmung der inneren Spannungnach der Stoney-GleichungThis Technical Specification (CEN/TS) wa
11、s approved by CEN on 8 August 2005 for provisional application.The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit theircomments, particularly on the question whether the CEN/TS can be converted into a European Sta
12、ndard.CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS availablepromptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)until the final decisio
13、n about the possible conversion of the CEN/TS into an EN is reached.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norwa
14、y, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any me
15、ans reservedworldwide for CEN national Members.Ref. No. CEN/TS 1071-11:2005: ELicensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSI2 Contents Page Foreword 3 1 Scope .4 2 Normative references .4 3 Principle.4 4 Apparatus 5 5 Preparation of test specimens .6 6 Pr
16、ocedure 6 7 Limits to method .9 8 Test report .10 Annex A (informative) Determination of suitable dimensions for the test sample11 Bibliography.13 CEN/TS 1071-11:2005Licensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSI3 Foreword This CEN Technical Specification
17、 (CEN/TS 1071-11:2005) has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, the secretariat of which is held by BSI. EN 1071 Advanced technical ceramics Methods of test for ceramic coatings consists of 11 parts: Part 1: Determination of coating thickness by contact prob
18、e filometer 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 composition by electron probe microanalysis (EPMA) Part 5: Determination of porosity Part 6: D
19、etermination of the abrasion resistance of coatings by a micro-abrasion wear test Part 7: Determination of hardness and Youngs modulus by instrumented indentation testing Part 8: Rockwell indentation test for evaluation of adhesion Part 9: Determination of fracture strain Part 10: Determination of c
20、oating thickness by cross sectioning Part 11: Measurement of internal stress by the Stoney formula Parts 5 to 6 are European prestandards. Parts 7 to 11 are Technical Specifications. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries ar
21、e bound to announce this CEN Technical Specification: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switze
22、rland and United Kingdom. CEN/TS 1071-11:2005Licensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSI4 1 Scope This Technical Specification specifies a method for the determination of the internal stress in thin ceramic coatings by application of the Stoney formula
23、 to the results obtained from measurement of the radius of curvature of coated strips or discs. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest e
24、dition of the referenced document (including any amendments) applies. EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 3 Principle Coating stress often plays a major role in the performance of coated tools and machine parts. Diffe
25、rent techniques have been developed for the determination of coating stress. The technique considered in this document calculates the stress from measurement of the bowing of thin discs or strips of well characterised materials of known thickness that have been coated on one side only. It is assumed
26、 that the deformation is elastic, i.e. if the coating were to be removed, the substrate would return to its initial shape. Provided that the coating is thin compared to the thickness of the substrate (coating thickness 20 m) radii of curvature using optical techniques. Before measuring the initial p
27、rofile, define a measuring range (length ), along the length a of the substrate (along a diameter for the disc). NOTE 1 In order to avoid any edge effects, the measuring range should stop at a distance from the ends equal to at least 20 times the sample thickness. CEN/TS 1071-11:2005Licensed Copy: W
28、ang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSI7 Make some reference marks, e.g. Vickers indentations, on the substrate, so that the final profile can be measured at the same location and in the same direction as the initial one. This procedure is essential when the initi
29、al profile is somewhat different from a perfect circle. NOTE 2 It is recommended that, where hardness indents are used as reference marks, indentations should be produced using a micro-hardness tester at a load of no greater than 1 kg. For measuring the profile, the sample shall lie freely, without
30、any external stress. Place the strip on two supports, so that it overhangs each support by a quarter of its length; proceed similarly for a disc. NOTE 3 In many cases supporting the sample on its ends will have negligible effect upon the curvature. However, the use of supports will avoid problems wi
31、th stability of the sample if one or both ends of the sample are not perpendicular to the sides. NOTE 4 Especially for thin samples, ensure that the weight of the sample does not change its shape: turning the strip (or disc) over on the supports should leave the profile unchanged, except for the sig
32、n. In the case of optical microscopy, measure accurately for each profile the coordinates ),(iizx of about ten points distributed uniformly along the predefined measuring range. The ordinate iz corresponds to the vertical position of the microscope objective for which the point ix of the surface of
33、the sample is in the image plane. The focusing axis of the microscope shall be perpendicular to the surface to be coated, and especially to its longitudinal axis see Figure 1. The initial curvature can be disregarded in so far as it is very low (R ) usually allows use of the simple method that consi
34、sts in approximating the arc of the circle to a parabola, i.e. 2210)( xMxMMxzR+= . The measured radius of curvature then is )2(12expMR = . NOTE 2 The profile is close to a circle if the radius of curvature is approximately constant along the profile. For verifying it, in the case where the profile i
35、s represented for instance by ten points, i. e. (iizx , ; i = 1 to 10), compare the radii of curvature obtained on considering the points i = 1 to i = 5, then i = 3 to i = 8, and then i = 5 to i = 10. The various radii should be nearly equal (A.2) EXAMPLE For a low strength steel substrate (y = 220
36、MPa and E = 220 GPa) 1 mm thick, plastic deformation occurs for radii of curvature lower than 0,5 m. NOTE In the case of coatings deposited with substrate heating and/or submitted to high temperature annealing, it is important to note that residual stresses exert their effect on a material with Eyra
37、tios different from those determined at room temperature. The Eyratio is not constant with temperature increase, with y usually being observed to decrease more strongly than E with an increase in the testing temperature. The order of magnitude to be chosen for hsis deduced through the Stoney formula
38、, where R is in the order of 1 m: ofsssRhEh =162(A.3) The length a of the strip (usually between 40 mm and 80 mm) determines the length of the measured profile ( is a little smaller than a , see 6.1). For measurement uncertainty in the order of z along the z direction, the condition to be verified i
39、s: a zR10 (A.4) CEN/TS 1071-11:2005Licensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSI12 The width b (a/b 10) should be low in order to minimise the non-linear effects relative to geometry. The corresponding condition is as follow: hRb22 1 (A.5) i.e. ()3216hEb
40、hsfos 1 (A.6) For a disc (diameter d ): hRd22 1 (A.7) From these various formulae, suitable dimensions for the test sample and coating thickness can be determined. However, if no order of magnitude value for the intrinsic stress in the coating is available, it will be necessary to make a preliminary
41、, approximate measurement using a suitable test specimen. CEN/TS 1071-11:2005Licensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSI13 Bibliography 1 EN 1071-1, Advanced technical ceramics Methods of test for ceramic coatings Part 1: Determination of coating thick
42、ness by contact probe filometer 2 EN 1071-2, Advanced technical ceramics Methods of test for ceramic coatings Part 2: Determination of coating thickness by the crater grinding method 3 CEN/TS 1071-10, Advanced technical ceramics Methods of test for ceramic coatings Part 10: Determination of coating
43、thickness by cross sectioning 4 Stoney, G G, Proc Roy Soc, A82 (1909) 172. 5 EN ISO 3274, Geometrical Product Specification (GPS) Surface texture: Profile method Nominal characteristic of contact (stylus) instruments (ISO 3274:1996) 6 DIN 50992-1:2002, Thickness measurement of coatings and character
44、ising of surfaces with surface waves Part 1: Evaluation of elastic constants, mass density and thickness of layers by laser-inducted ultrasonic surface waves 7 A S Maxwell, S Owen-Jones and N M Jennett, Measurement of Youngs modulus and Poissons ratio of thin coatings using impact excitation and dep
45、th sensing indentation, Rev. Sci. Instruments, 75, No. 4, April 2004. 8 Measurement Note MATC (MN) 51, Measurement of the Poissons ratio of coatings, National Physical Laboratory, UK, June 2003. 9 A. Brenner and S. Senderoff, J. Res. Nat. Bur. Stand., 42 (1949) 105. 10 L.B. Freund, J.A. Floro, E. Ch
46、ason, Extensions of the Stoney formula for substrate curvature to configurations with thin substrates or large deformations, Applied Physics Letters, 1999, 74(14), 1987-1989). CEN/TS 1071-11:2005Licensed Copy: Wang Bin, na, Tue Mar 27 06:04:40 GMT+00:00 2007, Uncontrolled Copy, (c) BSIDD CEN/TS 1071
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