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、3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 1071-11:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 31 January 2007 BSI 2007ISBN 978-0-580-49935-7National forewordThis Draft for Devel
3、opment 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 publications and is of a provisional nature. It should be applied on this provisional basis, so that
4、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 organization responsible for its conversion to a European standard. A review of this publication wil
5、l 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 announcement in the appropriate issue of Update Standards.According to the replies received by the
6、 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 should be sent to the Secretary of the responsible BSI Technical Committee at British Standar
7、ds 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 can be obtained on request to its secretary.This publication does not purport to include all
8、the necessary provisions of a contract. Users are responsible for its correct application.Amendments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 1071-11October 2005ICS 81.060.30English VersionAdvanced technical ceramics -
9、Methods of test for ceramiccoatings - Part 11: Determination of internal stress by theStoney formulaCramiques techniques avances - Mthodes dessaispour revtements cramiques - Partie 11 :Dtermination dela contrainte interne par la formule de StoneyHochleistungskeramik - Verfahren zur Prfung keramische
10、rSchichten - Teil 11: Bestimmung der inneren Spannungnach der Stoney-GleichungThis Technical Specification (CEN/TS) was 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 r
11、equested to submit theircomments, particularly on the question whether the CEN/TS can be converted into a European Standard.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
12、. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)until the final decision 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, Finla
13、nd, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMU
14、NGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. CEN/TS 1071-11:2005: E2 Contents Page Foreword 3 1 Scope .4 2 Normative references .4 3 Principle.4 4 Apparatus 5 5 Preparatio
15、n of test specimens .6 6 Procedure 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 1071-11:20053 Foreword This CEN Technical Specification (CEN/TS 1071-11:2005) has been prepared by Technical Committee
16、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 probe filometer Part 2: Determination of coating thickness by the cr
17、ater 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: Determination of the abrasion resistance of coatings by a micro-a
18、brasion 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 coating thickness by cross sectioning Part 11: Measurement of int
19、ernal 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 are bound to announce this CEN Technical Specification: Austria, B
20、elgium, 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, Switzerland and United Kingdom. CEN/TS 1071-11:20054 1 Scope This Tech
21、nical Specification specifies a method for the determination of the internal stress in thin ceramic coatings by application of the Stoney formula to the results obtained from measurement of the radius of curvature of coated strips or discs. 2 Normative references The following referenced documents a
22、re 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. EN ISO/IEC 17025, General requirements for the competence of testing and calibration
23、laboratories (ISO/IEC 17025:2005) 3 Principle Coating stress often plays a major role in the performance of coated tools and machine parts. Different techniques have been developed for the determination of coating stress. The technique considered in this document calculates the stress from measureme
24、nt 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 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 thi
25、n compared to the thickness of the substrate (coating thickness 20 m) radii of curvature using optical techniques. Before measuring the initial profile, 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,
26、 the measuring range should stop at a distance from the ends equal to at least 20 times the sample thickness. CEN/TS 1071-11:20057 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 i
27、nitial one. This procedure is essential when the initial 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 measur
28、ing the profile, the sample shall lie freely, without 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 curvatur
29、e. However, the use of supports will avoid problems with 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
30、should leave the profile unchanged, except for the sign. 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 microsco
31、pe objective for which the point ix of the surface of 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 (
32、R ) usually allows use of the simple method that consists 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 prof
33、ile. For verifying it, in the case where the profile is 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
34、) EXAMPLE For a low strength steel substrate (y = 220 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 residu
35、al stresses exert their effect on a material with Eyratios 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
36、 be chosen for hsis deduced through the Stoney formula, 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
37、 along the z direction, the condition to be verified is: a zR10 (A.4) CEN/TS 1071-11:200512 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. ()3216hEbhsfos 1 (A.6) For a disc (diameter d
38、): 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, approximate measurement using a sui
39、table test specimen. CEN/TS 1071-11:200513 Bibliography 1 EN 1071-1, Advanced technical ceramics Methods of test for ceramic coatings Part 1: Determination of coating thickness by contact probe filometer 2 EN 1071-2, Advanced technical ceramics Methods of test for ceramic coatings Part 2: Determinat
40、ion 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 thickness by cross sectioning 4 Stoney, G G, Proc Roy Soc, A82 (1909) 172. 5 EN ISO 3274, Geometrical Product Specification (GPS
41、) Surface texture: Profile method Nominal characteristic of contact (stylus) instruments (ISO 3274:1996) 6 DIN 50992-1:2002, Thickness measurement of coatings and characterising of surfaces with surface waves Part 1: Evaluation of elastic constants, mass density and thickness of layers by laser-indu
42、cted 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 depth sensing indentation, Rev. Sci. Instruments, 75, No. 4, April 2004. 8 Measurement Note MATC (MN) 51, Measurement of the Poisso
43、ns 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. Chason, Extensions of the Stoney formula for substrate curvature to configurations with thin substrates or large deformations, App
44、lied Physics Letters, 1999, 74(14), 1987-1989). CEN/TS 1071-11:2005DD CEN/TS 1071-11:2005BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the i
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