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The paper addresses the “State-of-the-Art in Multiple-Sample Evaluation of Adhesive and Bonding Strength” and the following points are discussed in more detail:
1. Motivation (coatings, varnishes, tapes, laminates, CFRP, adhesive-bonded joints)
2. Conventional single-sample testing (evaluation of adhesive and bonding strength; failure pattern)
3. Multiple-sample handling (MSH), bonding (MSB), and testing: centrifugal adhesion testing (CAT) (multiple-sample approach, tensile test within a centrifuge)
4. Application examples of CAT-Technology™ (laminates, optical coatings, CFRP joints)
Finally, a summary is given regarding status quo and benefits of CAT-technology under tensile stress conditions whereas examples of testing in a centrifuge under compressive stress conditions are mentioned in the outlook.
Bonding strength is crucial on polymers of low surface energy, for clean surfaces limited to 0.5, 1, and 2 MPa for PTFE, PP, and PE. Plasma treatment may improve bonding strength by a factor of 2 (PTFE) or 5 (PP and PE). The efficiency of treatment is usually 10% as both low pressure and atmospheric pressure processes show low topographic conformity.
Besides, lifetime of activation/modification is rather short. Hence, bonding has to be carried out immediately after plasma treatment.
The concept of plasma-assisted ALD (atomic layer deposition) interlayers was introduced in the project HARFE of SENTECH (modification/deposition/in-situ monitoring) and BAM (bonding, characterization, testing). ALD deposition has a high surface conformity and for dielectric films of Al2O3 also a good long-term stability given that the films are dense enough.
Based on TMA and O2/O3 precursors, ALD layer stacks from 60 to 375 monolayers were prepared under different conditions. For a transfer time of 24 hours from deposition to measurement, bonding strength could be increased up to 5 MPa (PTFE) respectively 10 MPa (PP, PE). The huge potential of ALD layers as adhesive interlayers was demonstrated for Al2O3 on stainless steel with bonding strength beyond 15 MPa, i.e. interface
strength within the ALD stack is also in this range.
This is a prerequisite for subsequent PVD/CVD-deposition in hybrid systems. By means of the SI ALD LL system of SENTECH thermal and plasma-supported ALD processes can be alternatively realized.
Ellipsometric in-situ monitoring provides monolayer sensitivity and reveals that the efficient bonding of the lower ALD layers on the polymer has to be further improved. Testing of bonding strength was realized by CAT (centrifugal adhesion testing) technology. It was shown that ALD modification correlates with the increase of surface energy and bonding strength.
The quantitative determination of adhesion and cohesion properties is a key requirement for adhesive-bonded joints and coated components in both R&D and Quality assurance. Because of the huge variety of layer/substrate Systems in terms of materials and large thickness range, adhesion tests display the same diversity as layer/substrate systems. There are only two tensile testing procedures available, that determine adhesive strength in terms of force per area (N/mm²), the single-sample pull-off test in a tensile testing machine and the multiple-sample-test using the Centrifugal Adhesion Testing (CAT) Technology.
The CAT Technology is a testing method which uses centrifugal force as tensile testing force in a multiple-sample arrangement within a drum rotor of a Desktop centrifuge. Hence, the adhesive/bonding strength A/B can be determined on a statistical basis under identical testing conditions for up to eight samples.
A variety of examples for bonding strength of adhesives, adhesive strength of coatings and compound strength of composite materials is discussed such as metalto-metal and glass-to-metal bonding, sputtered SiO2-layers on CR39 Polymer and carbon fiber reinforced polymer.
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.
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.
The quality and durability of bonded joints, coated systems and composites depend on various factors. Therefore effective quantitative tests to determine adhesive, bonding or composite strength are of great need for R&D and QC. In this paper a new measuring principle is described which uses the centrifugal force to generate the test load. By the geometry of the whole measurement set-up, the test specimen are supported from only one side, the influence of shear forces is avoided. The possibility to test up to eight samples in one measurement under identical testing conditions allows a high sample throughput.
A detailed description of the whole sample preparation procedure including pre-treatment is followed by the specification of the measuring protocol as well as result analysis. For each application area bonding strength of joints, adhesive strength of coated systems and internal strength of composite materials examples are presented.
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.
Sufficient adhesion/tensile strength are basic requirements for any coating/composite material. For coatings, adhesive strength in N/mm2 is of Major interest for various applications such as decorative and water-repellent coatings on wood (paints and varnishes), optical coatings on glass and polymers (reflectors and filters), electrical coatings on semiconductors, glass and polymers (conducting and bondable layers), mechanical coatings on metals and polymers (wear-reduction, scratch-resistance) and adhesion-promoting layers. For composite materials, tensile strength in N/mm2 is also a key quantity for carbon fiber reinforced composites (CFC), laminates and adhesive-bonded joints. Centrifugal adhesion testing (CAT) transfers the single-sample tensile test from a tensile or universal testing machine into an analytical centrifuge as multiple-sample test of up to eight test pieces. The one-sided sample support instead of a two-sided sample clamping and the absence of mounting- and testing-correlated shear forces provides fast and reliable results both for adhesive strength and bonding strength by means of bonded test stamps. For bonding strength, the evaluation of failure pattern from microscopic inspection is required in order to determine the failure pattern according to ISO 10365 such as adhesive failure (AF), delamination failure (DF) and cohesive failure (CF). Hence, one test run by CAT-technology provides either statistics or ranking of up to eight samples at once. For adhesive strength of coatings, a variety of examples is discussed such as ALD-Al203 layers as adhesion promoters, evaporated Ag-layers on N-BK7 glass, sputtered Cr- and Al-layers on Borofloat 33 glass, evaporated Au-films on N-BK7 glass and sputtered SiO2 -layers on CR39 Polymer. Provided adhesive or bonding strength are high enough, the substrate or the joining part may also fail.