BS-EN-ISO-14577-4-2007.pdf

BRITISH STANDARD BS EN ISO 14577-4:2007 Metallic materials Instrumented indentation test for hardness and materials parameters Part 4: Test method for metallic and non-metallic coatings The European Standard EN ISO 14577-4:2007 has the status of a British Standard ICS 77.040.10 ? Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN ISO 14577-4:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 29 June 2007 © BSI 2007 ISBN 978 0 580 53802 5 National foreword This British Standard was published by BSI. It is the UK implementation of EN ISO 14577-4:2007. The UK participation in its preparation was entrusted by Technical Committee ISE/NFE/4, Mechanical testing of metals, to Subcommittee ISE/NFE/4/5, Indentation hardness testing. A list of organizations represented on this committee can 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. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 14577-4 May 2007 ICS 77.040.10 English Version Metallic materials - Instrumented indentation test for hardness and materials parameters - Part 4: Test method for metallic and non-metallic coatings (ISO 14577-4:2007) Matériaux métalliques - Essai de pénétration instrumenté pour la détermination de la dureté et de paramètres des matériaux - Partie 4: Méthode d'essai pour les revêtements métalliques et non métalliques (ISO 14577-4:2007) Metallische Werkstoffe - Instrumentierte Eindringprüfung zur Bestimmung der Härte und anderer Werkstoffparameter - Teil 4: Prüfverfahren für metallische und nichtmetalische Schichten (ISO 14577-4:2007) This European Standard was approved by CEN on 13 April 2007. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions 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 official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, 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 FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels © 2007 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14577-4:2007: E Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI Foreword This document (EN ISO 14577-4:2007) has been prepared by Technical Committee ISO/TC 164 “Mechanical testing of metals“ in collaboration with Technical Committee ECISS/TC 1 “Steel - Mechanical testing“, the secretariat of which is held by AFNOR. 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 November 2007, and conflicting national standards shall be withdrawn at the latest by November 2007. 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 14577-4:2007 has been approved by CEN as EN ISO 14577-4:2007 without any modifications. EN ISO 14577-4:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI Reference number ISO 14577-4:2007(E) INTERNATIONAL STANDARD ISO 14577-4 First edition 2007-05-15 Metallic materials Instrumented indentation test for hardness and materials parameters Part 4: Test method for metallic and non-metallic coatings Matériaux métalliques Essai de pénétration instrumenté pour la détermination de la dureté et de paramètres des matériaux Partie 4: Méthode d'essai pour les revêtements métalliques et non métalliques EN ISO 14577-4:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI ii Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references. 1 3 Symbols and designations 2 4 Verification and calibration of testing machines. 2 5 Test pieces 4 5.1 General. 4 5.2 Surface roughness . 4 5.3 Polishing 5 5.4 Surface cleanliness 5 5.5 Special requirements for paints and varnishes. 5 6 Procedure 6 6.1 Test conditions . 6 6.2 Measurement procedure 9 7 Data analysis and evaluation of results for indentation normal to the surface. 11 7.1 General. 11 7.2 Coating indentation modulus 12 7.3 Coating indentation hardness. 13 8 Test report . 16 Annex A (normative) Frame compliance calibration procedure . 17 Annex B (normative) Contact point and fully elastic regime. 21 Bibliography. 23 EN ISO 14577-4:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 14577-4 was prepared by Technical Committee ISO/TC 164, Mechanical testing of metals, Subcommittee SC 3, Hardness testing. ISO 14577 consists of the following parts, under the general title Metallic materials Instrumented indentation test for hardness and materials parameters: Part 1: Test method Part 2: Verification and calibration of testing machines Part 3: Calibration of reference blocks Part 4: Test method for metallic and non-metallic coatings EN ISO 14577-4:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI v Introduction The elastic and plastic properties of a coating are critical factors determining the performance of the coated product. Indeed many coatings are specifically developed to provide wear resistance that is usually conferred by their high hardness. Measurement of coating hardness is often used as a quality control check. Youngs modulus becomes important when calculation of the stress in a coating is required in the design of coated components. For example, the extent to which coated components can withstand external applied forces is an important property in the capability of any coated system. It is relatively straightforward to determine the hardness and indentation modulus of bulk materials using instrumented indentation. However, when measurements are made normal to a coated surface, depending on the force applied and the thickness of the coating, the substrate properties influence the result. The purpose of this part of ISO 14577 is to provide guidelines for conditions where there is no significant influence of the substrate, and, where such influence is detected, to provide possible analytical methods to enable the coating properties to be extracted from the composite measurement. In some cases, the coating property can be determined directly from measurements on a cross-section. EN ISO 14577-4:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI blank Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 1 Metallic materials Instrumented indentation test for hardness and materials parameters Part 4: Test method for metallic and non-metallic coatings 1 Scope This part of ISO 14577 specifies a method for testing coatings which is particularly suitable for testing in the nano/micro range applicable to thin coatings. This test method is limited to the examination of single layers when the indentation is carried out normal to the test piece surface, but graded and multilayer coatings can also be measured in cross-section if the thickness of the individual layers or gradations is greater than the spatial resolution of the indentation process. The test method is not limited to any particular type of material. Metallic, non-metallic and organic coatings are included in the scope of this part of ISO 14577. The application of this part of ISO 14577 regarding measurement of hardness is only possible if the indenter is a pyramid or a cone with a radius of tip curvature small enough for plastic deformation to occur within the coating. The hardness of visco-elastic materials, or materials exhibiting significant creep will be strongly affected by the time taken to perform the test. NOTE 1 ISO 14577-1, ISO 14577-2 and ISO 14577-3 define usage of instrumented indentation testing of bulk materials over all force and displacement ranges. NOTE 2 The application of the method of this part of ISO 14577 is not needed if the indentation depth is so small that in any possible case a substrate influence can be neglected and the coating can be considered as a bulk material. Limits for such cases are given. NOTE 3 The analysis used here does not make any allowances for pile-up or sink-in of indents. Use of Atomic Force Microscopy (AFM) to assess the indent shape allows the determination of possible pile-up or sink-in of the surface around the indent. These surface effects result in an under-estimate (pile-up) or over-estimate (sink-in) of the contact area in the analysis and hence may influence the measured results. Pile-up generally occurs for fully work-hardened materials. Pile- up of soft, ductile materials is more likely for thinner coatings due to the constraint of the stresses in the zone of plastic deformation in the coating. It has been reported that the piled up material results in an effective increase of the contact area for the determination of hardness, while the effect is less pronounced for the determination of indentation modulus, since the piled up material behaves less rigidly 1, 2. 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 edition of the referenced document (including any amendments) applies. ISO 1514, Paints and varnishes Standard panels for testing ISO 2808, Paints and varnishes Determination of film thickness ISO 3270, Paints and varnishes and their raw materials Temperatures and humidities for conditioning and testing EN ISO 14577-4:2007 Licensed Copy: London South Bank University, London South Bank University, Tue Jul 03 00:59:05 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 2 ISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parameters ISO 14577-1:2002, Metallic materials Instrumented indentation test for hardness and materials parameters Part 1: Test method ISO 14577-2, Metallic materials Instrumented indentation test for hardness and materials parameters Part 2: Verification and calibration of testing machines ISO 14577-3, Metallic materials Instrumented indentation test for hardness and materials parameters Part 3: Calibration of reference blocks 3 Symbols and designations The symbols and designations in ISO 14577-1, ISO 14577-2 and ISO 14577-3 and in Table 1 apply. Table 1 Symbols and designations Symbol Designation Unit Required in the test report F Test force mN ? Ap(hc) Projected area of contact of the indenter at distance hc from the tip µm2 Hc Indentation hardness of the coating mN/µm2 b ? i Poisson's ratio of the indenter a s Poisson's ratio of the test piece a Radius of contact area µm tc Film thickness µm ? Cf Frame compliance µm/mN ? Cs Contact compliance (test piece) µm/mN Ct Total measured compliance µm/mN E Young's modulus mN/µm2 b Ec* Plane strain indentation modulus of the coating c mN/µm2 EIT* Plane strain indentation modulus mN/µm2 b ? Er Reduced modulus of the indentation contact mN/µm2 b Ra Arithmetic mean deviation from the average height of the assessed profile (see ISO 4287). µm a For diamond i = 0,07. b 1 mN/µm2 = 1 GPa. c Ec* = EIT* (at a/tc = 0). 4 Verification and calibration of testing machines The instrument shall be calibrated according to the procedures set out in ISO 14577-2 and Annex A. Indirect verification using a reference material shall be made to ensure th