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Multiple-sample approach: reliable ranking and validated statistics of bonding and adhesive strength
(2014)
Bonding strength of adhesive-bonded joints and adhesive strength of coatings have been exclusively determined in
single-sample tests using a tensile testing machine. Necessarily, the single-sample approach was also applied to the
corresponding bonding procedure. As a consequence, reliability and reproducibility of results were restricted. By
applying the newly introduced centrifuge technology, the multiple-sample approach was realized for simultaneous
tensile testing of up to eight samples under identical conditions without any disturbing shear-force effects. In order to
introduce the multiple-sample approach into the bonding procedure, a hydraulic bonding set-up was developed which
enables identical bonding pressure also for slightly different heights of sample assemblies. Both sample approaches
were compared for various application examples: ranking of different classes of adhesives, validated statistics of
adhesive-bonded joints using one particular adhesive and effects of cleaning and plasma-treatment on the adhesive
strength of coatings. The investigated systems included glass, metals and polymer substrates, different adhesives,
metallic and dielectric coatings on polymers.
Although adhesion testing of coatings is of fundamental interest for quality assurance, it is still a challenge regarding reliable quantitative results. Because of the huge variety of coating/ substrate systems in terms of materials and thickness range, adhesion tests display the same variety as coating/substrate systems. Some tests are qualitative, many are quantitative but except for the pull (DIN EN ISO 15870) and pull-off test (DIN EN ISO 4624) adhesion is not measured in terms of force per area.
For optical coatings, the standardized tests according to ISO 9211-4 apply, i.e. abrasion tests (cheese cloth or eraser test) and adhesion tests (tape or cross-hatch test) with different degrees of severity. Instead of the adhesion strength, all these single-sample tests provide only quantitative information on the abrasion or adhesion resistance of a particular coating/ substrate system.
The centrifuge test has manifold advantages. First, it can be easily run as multiple-sample test. Second, adhesion strength is measured in absolute numbers (N/mm2). Third, the centrifuge test requires only a one-sided sample support instead of a two-sided sample clamping as the pull- and pull-off test do. Fourth, it is much easier and faster than many other tests. Fifth, the centrifuge technology additionally enables tests under defined climates or harsh environments. Last but not least, versatile test conditions (alternating loads at various load rates) important to fatigue testing can be easily realized by varying the number of revolutions.
The centrifuge test was applied to the testing of optical coatings on glass and CaF2. It could be shown that there are significant advantages compared to other tests. In particular, the centrifuge test was able to discriminate the adhesion strength for coating/substrate systems until failure which all passed the standardized tests of ISO 9211-4.
A new technology for strength determination of adhesive-bonded joints based on analytical centrifugatioon is introduced. Tensile as well as shear strength can be measured for multiple test specimens simultaneously within a very short time. The experimental procedure is described from sample preparation, application of adhesives, sample mounting within the centrifuge to testing parameters and sequences. All requirements of DIN EN 15870 are fulfilled and, in addition, a higher throughput and a better reproducibility can be obtained. The experimental results are discussed regarding bonding strength development over time, comparison of tensile and shear strength and various testing conditions. Furthermore, an additional application field of centrifuge technology is described with respect to the determination of the adhesive strength of coatings. The novel centrifuge based technology provides the determination of bonding, adhesive and shear strength on a statistical basis under identical testing conditions for up to eight samples. Moreover, sophisticated two-sided sample clamping, necessary for a tensile testing machine, is replaced by a simple plug-in procedure.