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1、INTERNATIONAL STANDARD ISO 4624 Second edition 2002-02-01 Reference number ISO 4624:2002(E) ISO 2002 Paints and varnishes Pull-off test for adhesion Peintures et vernis Essai de traction ISO 4624:2002(E) ii ISO 2002 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In
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4、printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2002 All rights reserved. Unless otherwise specified, no part of t
5、his publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1
6、211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland -,-,- ISO 4624:2002(E) ISO 2002 All rights reserved iii Contents Page 1Scope . 1 2Normative references . 1 3Principle 1 4Required supplementary information . 2 5Apparatus . 2 6Adhe
7、sives . 4 7Sampling . 4 8Test panels . 5 9Procedure . 5 10Calculation and expression of results . 8 11Precision . 8 12Test report 9 Annex ARequired supplementary information 10 Bibliography. 11 ISO 4624:2002(E) iv ISO 2002 All rights reserved Foreword ISO (the International Organization for Standard
8、ization) 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
9、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 Stand
10、ards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. 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 ca
11、sting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 4624 was prepared by Technical Committee ISO/T
12、C 35, Paints and varnishes, Subcommittee SC 9, General test methods for paints and varnishes. This second edition cancels and replaces the first edition (ISO 4624:1978), clause 6 and subclauses 5.1, 5.2, 5.4 and 8.2 of which have been technically revised. Annex A forms a normative part of this Inter
13、national Standard. ISO 4624:2002(E) ISO 2002 All rights reserved v Introduction This International Standard is one of two standards which describe methods for assessing the adhesion of a single coating or a multi-coat system of paint, varnish or related product by measuring the minimum tensile stres
14、s necessary to detach or to rupture the coating in a direction perpendicular to the substrate. The test result is influenced not only by the mechanical properties of the system under test, but also by the nature and preparation of the substrate, the method of paint application, the drying conditions
15、 of the coating, the temperature, the humidity and other factors like the type of test instrument which has been used. The other International Standard is ISO 2409:1992, Paints and varnishes Cross-cut test. INTERNATIONAL STANDARDISO 4624:2002(E) ISO 2002 All rights reserved 1 Paints and varnishes Pu
16、ll-off test for adhesion 1Scope This International Standard describes methods for determining the adhesion by carrying out a pull-off test on a single coating or a multi-coat system of paint, varnish or related product. These test methods have been found useful in comparing the adhesion behaviour of
17、 different coatings. It is most useful in providing relative ratings for a series of coated panels exhibiting significant differences in adhesion. The test may be applied using a wide range of substrates. Different procedures are given according to whether the substrate is deformable, for example th
18、in metal, plastics and wood, or rigid, for example thick concrete and metal plates. For special purposes, the coating may be applied directly to the face of a test dolly. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute prov
19、isions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of th
20、e normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 1513:1992, Paints and varnishes Examination and preparation of samples for testin
21、g ISO 1514:1), Paints and varnishes Standard panels for testing ISO 2808:1997, Paints and varnishes Determination of film thickness ISO 3270:1984, Paints and varnishes and their raw materials Temperatures and humidities for conditioning and testing ISO 15528:2000, Paints, varnishes and raw materials
22、 for paints and varnishes Sampling 3Principle The product or system under test is applied at uniform thickness to flat panels of uniform surface texture. After drying/curing the coating system, dollies are bonded directly to the surface of the coated, cured panel using an adhesive. After curing of t
23、he adhesive, the bonded dolly assemblies are placed in a suitable tensile tester. The bonded assemblies are subjected to a controlled tensile test (pull-off test), and the force required to break the coating/substrate bond is measured. The test result is the tensile stress necessary to break the wea
24、kest interface (adhesive failure) or the weakest component (cohesive failure) of the test assembly. Mixed adhesive/cohesive failures may also occur. 1)To be published. (Revision of ISO 1514:1993) -,-,- ISO 4624:2002(E) 2 ISO 2002 All rights reserved 4Required supplementary information For any partic
25、ular application, the test methods specified in this International Standard need to be completed by supplementary information. The items of supplementary information are given in annex A. 5Apparatus 5.1Tensile tester, suitable for carrying out the chosen procedure specified in clause 9. The tensile
26、stress shall be applied in a direction perpendicular to the plane of the coated substrate and shall be increased at a substantially uniform rate, not greater than 2), such that failure of the test assembly occurs within . Suitable designs for applying the tensile stress are shown in Figures 1 and 2.
27、 NOTE 1Instead of a tensile tester, other types of pull-off adhesion testers (mechanically, pneumatically, hydraulically or hand- driven) may be used provided that they give similar results. The type of instrument shall be reported in the test report, because hand-driven/mechanical/hydraulic instrum
28、ents are reported to produce widely different results. NOTE 2The results can be influenced by the test assembly used. Furthermore, the results are not reproducible unless coaxial alignment of the tensile forces is ensured. 2) Key 1Support 2Ball joint 3Dollies 4Coating 5Substrate Figure 1 Example of
29、a suitable test apparatus for the methods described in 9.4.1 and 9.4.3 1 MPa/s90 s 1 MPa/s=1 MN/m2s -,-,- ISO 4624:2002(E) ISO 2002 All rights reserved 3 5.2Test dollies, each consisting of a steel- or aluminium-faced cylinder, specifically designed to be used with the tensile tester. Each dolly has
30、 a rigid, flat face for bonding the adhesive/coating at one end and a facility for connecting the pull-off tester at the other. Each dolly has a nominal diameter of (see however following paragraph) and sufficient thickness to ensure freedom from distortion during the test. It is recommended that th
31、e length of each dolly is not less than half its diameter. The faces of each dolly shall be machined perpendicular to its axis before use. Dollies with a diameter of may be used when the method for testing adhesion from one side only is used (see 9.4.2). If dollies of in diameter are used, 10 measur
32、ements shall be made to improve the precision. The diameter of the dollies shall be reported in the test report. 5.3Centering device, for ensuring proper coaxial alignment of the test assembly during the adhesion process described in 9.4.1 and 9.4.3. A suitable design is shown in Figure 3. 5.4Cuttin
33、g device, such as a sharp knife, for cutting through cured adhesive and the paint coating to the substrate, round the circumference of the dolly. Depending on the mechanical properties of the paint system (e.g. brittleness), cutting through the cured adhesive and the paint film to the substrate can
34、have a big influence on the adhesion of the paint system. It is permitted, if specified or agreed between the interested parties, not to cut when the paint systems are less than in layer thickness. If cuts around the dolly have been made, this shall be mentioned in the test report and the type of cu
35、tting tool also mentioned. Key 1Coating 2Test piece 3Dolly 4Ball-and-socket sliding joint 5Support (suitably designed to allow for joint assembly) 6Ball-and-socket sliding joint Figure 2 Example of a suitable test apparatus for the method described in 9.4.2 20 mm 7 mm 7 mm 150m -,-,- ISO 4624:2002(E
36、) 4 ISO 2002 All rights reserved 6Adhesives Special attention is required in selecting suitable adhesives to be used in the test. To produce failure of the coating, it is essential that the cohesive and bonding properties of the adhesive are greater than those of the coating under test. Preliminary
37、screening of adhesives shall be carried out in order to determine their suitability for use. Suitable adhesives and, if applicable, their unmixed components shall cause little or no visible change in the coating under test when left in contact with the coating for a period equivalent to the curing t
38、ime of the adhesive. Adhesives which give the highest results, which means the most coating-substrate adhesive failure, are preferred. In most cases, cyanoacrylate, two-component solventless epoxide and peroxide-catalysed polyester adhesives have been found suitable. In special tests under highly hu
39、mid conditions, the curing time of the adhesive shall be as short as possible. The use of two-pack quick-drying epoxy adhesive is preferable in these situations. NOTEWhere failure is mainly associated with the adhesive, the use of another type of adhesive may enable more useful results to be obtaine
40、d. 7Sampling Take a representative sample of the product to be tested (or of each product in case of a multi-coat system), as described in ISO 15528. Examine and prepare the sample for testing, as described in ISO 1513. Dimensions in millimetres Key 1Test assembly aligned for adhesion process (see 5
41、.3) 2Centering pin Figure 3 Example of a suitable centering device for 20-mm-diameter dollies -,-,- ISO 4624:2002(E) ISO 2002 All rights reserved 5 8Test panels 8.1Substrate Unless otherwise agreed, select the substrate from one of those described in ISO 1514, using where possible the same type of m
42、aterial as will be used in practice. The substrate panels shall be plane and free from distortion. 8.2Preparation and coating Unless otherwise agreed, prepare each test panel in accordance with that pretreatment method which is intended to be carried out on the original surface. The chosen pretreatm
43、ent shall be reported in the test report. 8.3Drying and conditioning Dry (or stove) and age, if applicable, each coated test panel for the specified time and under the specified conditions. Before testing, condition the coated panels at and a relative humidity of (see ISO 3270), unless otherwise agr
44、eed, for a minimum period of 16 hours. 8.4Thickness of coating The thickness of the coating shall be specified and agreed between the interested parties. Determine the thickness, in micrometres, of the dried coating by one of the procedures specified in ISO 2808. NOTESee also clause 1. 9Procedure 9.
45、1Number of determinations Carry out at least six determinations, i.e. using at least six test assemblies (see 9.4). 9.2Ambient conditions Carry out the test at and a relative humidity of , unless otherwise agreed (see ISO 3270). 9.3Adhesive Prepare and apply the adhesive (see clause 6) in accordance
46、 with the manufacturers instructions. Use the minimum quantity of adhesive required to produce a firm, continuous and even bond between the components of the test assembly. Remove any excess adhesive immediately if possible. 9.4Test assemblies 9.4.1General method (using two dollies) for testing both
47、 rigid and deformable substrates Use as the test piece an area, cut from the coated substrate (disc of minimum diameter or square of minimum side ). Take care not to distort the test piece. Apply the adhesive evenly to the surfaces of two freshly-cleaned dollies (5.2) of equal diameter (see notes 1
48、and 2). Place the test piece between the adhesive-coated faces of the dollies such that the dollies are coaxially aligned in the centre of the test piece, as shown in Figure 4. Align the test assembly in the centering device (5.3) and maintain the alignment for a period equal to the curing time of the adhesive. In special tests under highly humid conditions, the (232) C (505)% (232) C (505)% 30 mm 30 mm ISO 4624:2002(E) 6 ISO 2002 All rights reserved curing time of the adhesive shall be as short as possible, the use of two-pack quick-drying epoxy adhesive is preferable in these situations. At