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User Benefits Application News Universal testing machine Copper foil peel test device Thermostatic chamber 10 mm 30 mm 100 mm 2 mm Substrate Plating seed layer Electrolytic copper plating (a) (b) Fig. 2 Instruments (a) Universal testing machine, Thermostatic chamber (b) Copper foil peel test device Testing machine : AGX-50NV2D Load cell : 50 N Jig : Copper foil peel test device Thermostatic chamber : Refrigerator thermostatic chamber, air-cooled type TCR2A Software : TRAPEZIUM X-V Fig. 1 Test Sample (a) Dimensions, (b) Cross section Fig. 1 shows the dimensions and cross section of the sample used in the measurement. Polybutylene terephthalate (PBT), which is a hard-to-plate resin, was used as the substrate. As a method for plating hard-to-plate resins, first, a thin plating seed layer is formed on the resin substrate as a conductive layer, and a plating of the specified thickness is then applied by an electroplating method. In this experiment, films with a thickness of approximately 0.6 μm were formed using two different methods of applying the plating seed layer (sputtering, which is a physical method, and electroless plating using a chemical reaction). After film-forming, a copper plating film with a target thickness of 25 μm was formed on the respective samples by the electroplating method. In the measurements, the plating layer was scribed with a cutter on a 10 mm part in the center of the 30 mm wide sample as the peel area. Test Sample Table 1 Sample Information Table 2 Instrument Configuration Fig. 3 Range of Data Used in Calculation of Adhesion The peel length is 60 mm or more. The adhesion of the plating was calculated from the average test force of the data taken from the length between the 10 mm and 60 mm after the start of peeling. (Fig. 3). The test width and speed of the test conditions were set referring to JIS H 8630, JIS C 6481, ASTM B 533-85 and ISO 25245. ISO 25245 specifies that the adhesion force shall be calculated using the 30 mm length from 10 mm to 40 mm after the start of peeling as valid data. Table 3 shows the test conditions. Parts produced by applying platings to the surface of resins are generally used in applications ranging from decorative parts in the automotive industry to electrical devices and the electrical and electronic/semiconductor fields. Since technologies for applying platings to hard-to-plate resins have also been required for the printed boards of automotive components and advanced electronic equipment in recent years, a wide-range of research and development projects are underway on topics including new resin materials, plating chemicals, and plating production processes. To ensure that plating films fully demonstrate their functions, films must secure adhesion without peeling under their intended use environments. At present, the main methods for evaluating the adhesion of plating are the thermal cycle test and the heat shock test, but these cannot be considered quantitative evaluation methods. This article introduces an example in which a peel test was conducted using a universal testing machine, and the adhesion of the plating under various temperature environments was quantified in accordance with ISO 25245. Introduction The adhesion of plating under temperature environments from -60 ˚C to 250 ˚C can be measured by using the jig and thermostatic chamber introduced in this article. It is possible to measure the adhesion of the plating as described in JIS H 8630, JIS C 6481 and ISO 25245. Peel Test of Plating Film on Resin Under Varied Temperature Environments with ISO 25245 Natsumi Koike, Hiroto Shimizu AGX -V2 Precision Universal Testing Machine Sample dimensions : Width 30 mm × length 100 mm × thickness 2 mm Substrate : Polybutylene terephthalate (PBT) Plating : Copper Seed layer film- forming methods : Sputtering Electroless plating (a) (b) 15 10 5 0 0 20 40 60 Stroke (mm) 80 Test force (N) Valid data range 50 mm Invalid data Invalid data 10 mm Test speed : 25 mm/min Set atmosphere temperatures : -50 ˚C, -25 ˚C, 0 ˚C, 25 ˚C, 50 ˚C, 75 ˚C, 100 ˚C, 125 ˚C Number of tests : N = 5 (at each set atmosphere temperature) Valid data range : 10 mm to 60 mm from start of peeling Peel width : 10 mm Table 3 Test Conditions The peel test was carried out using a universal testing machine and a thermostatic chamber. Fig. 2 shows views of the test, and Table 2 shows the instrument configuration. Instruments and Test Conditions
Application News www.shimadzu.com/an/ Shimadzu Corporation © Shimadzu Corporation, 2024 For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. See http://www.shimadzu.com/about/trademarks/index.html for details. Third party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “”. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. First Edition: Sep. 2024 Revision A: Sep. 2026 01-00703A-EN Test Results Conclusion AGX is a trademark of Shimadzu Corporation or its affiliated companies in Japan and/or other countries. Prior to the peel test, the relationship between the film thickness and adhesion of the plating was investigated. The film thickness in the central part of the samples was measured nondestructively by using the X-ray fluorescence method. Although the target film thickness of the plating in film-forming for this test was 25 μm, the measured values of the film thickness spanned a range from 15 μm to 30 μm. As the result of a room-temperature peel test of those specimens, Fig. 4 shows an adhesion-plating film thickness graph. The correlation coefficient of the film thickness and adhesion was 0.86, indicating that adhesion has a strong correlation with the film thickness of the plating. Thus, it can be said that measuring the plating film thickness and evaluating adhesion using specimens with approximately the same film thickness are important in quantitative evaluations of adhesion. To evaluate adhesion when the temperature environment was changed, a peel test was carried out using samples with measured plating film thicknesses from 20 μm to 25 μm. As an example of the results, Fig. 5 shows the test force-stroke graphs of samples prepared by the two different film deposition methods. Fig. 5 (a) shows the test results for the specimens when film- forming was done by the sputtering method, and (b) shows the results for the specimens prepared by electroless plating. A peel test of specimens prepared by applying copper platings to a hard-to-plate resin was conducted in a thermostatic chamber using an AGX-V2 precision universal testing machine in accordance with ISO 25245. It was found that the film thickness of the plating affected plating adhesion, and adhesion showed temperature dependence, tending to decrease at high temperatures exceeding 100 ˚C. Evaluation of adhesion under a wide range of temperature environments, assuming different use environments, is an effective test method for various types of development, including the development of film-forming methods for plating, resin materials, plating chemicals, and plating production process. <Acknowledgement> In the preparation of this Application News article, the authors received generous cooperation, including provision of test materials and instructions regarding the analysis conditions, from the Osaka Research Institute of Industrial Science and Technology (ORIST, a Local Incorporated Administrative Agency). We wish to express our heartfelt thanks to all those concerned. Fig. 4 Adhesion-Plating Film Thickness Relationship (Sputtering) Adhesion (N) Plating film thickness (μm) 15 10 5 0 0 10 20 30 40 8 4 2 0 6 0 20 40 60 80 Stroke (mm) Test force (N) (b) 15 10 5 0 (a) 0 20 40 60 80 Stroke (mm) Test force (N) Adhesion (average): 10.18 N Adhesion (average): 3.44 N Fig. 5 Test Force-Stroke Graphs (Room Temperature) (a) Sputtering, (b) Electroless plating Table 4 Test Results (Average Values) Temp. (˚C) (a) Sputtering (b) Electroless plating Adhesion (N) Difference (vs. 25 ˚C baseline) (%) Adhesion (N) Difference (vs. 25 ˚C baseline) (%) -50 12.33 21.10 4.25 23.63 -25 11.19 9.85 4.07 18.27 0 10.82 6.21 3.68 7.00 25 10.18 - 3.44 - 50 10.23 0.43 4.45 29.43 75 9.57 -6.08 4.31 25.39 100 9.35 -8.19 3.19 -7.32 125 8.99 -11.71 2.39 -30.49 -50 -25 0 100 125 25 50 75 0 5 10 15 (a) Sputtering (b) Electroless plating Adhesion (N) Temperature (˚C) Average value × Fig. 6 Adhesion-Temperature Relationship Table 4 shows the test results (average of N = 5 tests) for the various temperatures, and Fig. 6 shows the relationship between the plating adhesion and thermostatic chamber temperature for each seed layer. When the seed layer was applied by sputtering, the adhesion of the plating showed a decreasing tendency as the temperature increased, and with electroless plating, there was almost no change from -50 ˚C to 75 ˚C, and a decreasing tendency was observed at 100 ˚C and higher.
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