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- Adhesive strength (2)
- Bonding strength (2)
- Centrifuge technology (2)
- Coatings (2)
- Flammability (2)
- High pressure oxygen (2)
- Metallic materials (2)
- Multi-sample approach (2)
- 3D coherence scanning interferometry (CSI) (1)
- Adhesion (1)
Organisationseinheit der BAM
Functionality of optical systems requires optical coatings of
high quality which have to be adapted to the application in
terms of the performance of optical parameters such as
reflectivity (AR, low, defined, high), the substrate material of
interest (polymers, ceramics, and glass), the environmental
conditions (such as temperature or humidity), and the service
conditions (such spectral range and power density). Moreover,
in many cases, additional non-optical requirements have
to be met, including mechanical features such as scratch
resistance, hardness and modulus.
Consequently, thickness and overall uniformity requirements
are steadily increasing. In general, these demands can usually
not be achieved by a single film or coating. Instead, films with
specific design features (such as gradients), layer stacks and
multilayers are a prerequisite for high quality layers and their
reliability. For the development of such layer systems, a
versatile cluster deposition system consisting of three clusters
and a cluster-to-cluster handler has been designed. Besides a
PECVD cluster for DLC coatings, two PVD clusters implement
ion assisted electron beam evaporation and plasmabased
sputter technology. In addition to metallic films, preparation
of oxide and nitride optical coatings (SiO2, TiO2, Ta2O5,
ITO, Al2O3, TiN, AlN) in various process modifications (nonreactive,
partially reactive, full-reactive; rf-, dc-, mf- mode;
PEM control) has been carried out.
Within this paper, the effect of several process parameters on
layer quality (optical constants, density, and uniformity) is
discussed for selected applications examples (AR- and HR
coatings, applications at elevated temperatures and applications
of enhanced mechanical performance).
It has been shown that specific features of ion and plasma
assisted PVD processes, including ion-beam and plasma preand
post-treatment of substrates and layer systems, may
widen the application range and improve functionality features
of given coating/substrate systems.
Public, hidden, and forensic features either encoded or directly legible are used for authentication. Fabry-Perot layer stacks as information carriers in combination with imaging ellipsometry as optical read-out system provide all-in-one anti-counterfeiting capability that may establish the new security level 'encoded forensic'. Different layer designs are described with regard to all three security levels: public features (e.g. color and tilt effect) perceptible by the human eye, hidden features (e.g. spectroscopic response in the UV or IR), and forensic features (ellipsometric quantities Ψ and Δ as a function of wavelength λ and angle of incidence AOI). Physically uncloneable functions (PUF) could be realized as a result of a multi-material and a multi-parameter deposition approach as well as by means of specific design features of the Fabry-Perot layer stack. Hence, they are not subject to any reverse engineering strategies. Examples of stratified, micro-structured, and laser-modified Fabry-Perot layer systems are considered that may be used at all perception levels (e.g. human eye, bar code reader, and imaging ellipsometry) for authentication against product counterfeiting and related areas. --------------------------------------------------------------------------------------------------------------------
Zur Authentifizierung werden offene, versteckte und forensische Merkmale entweder codiert oder direkt auslesbar verwendet. Mit Fabry-Perot Schichtsystemen als Informationsträger in Kombination mit der abbildenden Ellipsometrie als optischem Auslesesystem steht ein 'all-in-one' Fälschungsschutz-System zur Verfügung, das ein neues Sicherheitsniveau 'kodiert-forensisch' darstellt. Es werden unterschiedliche Schichtdesigns beschrieben, mit denen alle drei Sicherheitsniveaus realisiert werden können: offene Merkmale (z.B. Farbe und Kippeffekt), die mit dem menschlichen Auge wahrnehmbar sind, versteckte Merkmale (z.B. die spektrale Antwort im Sichtbaren oder im IR) sowie forensische Merkmale (ellipsometrische Größen Ψ und Δ als Funktion der Wellenlänge λ und des Einfallswinkels AOI).
Physikalisch nicht klonbare Funktionen (PUF) können im Ergebnis einer Multi-Material- und Multi-Parameter Beschichtungsstrategie sowie durch spezifische Design-Merkmale des Fabry-Perot Schichtsystems realisiert werden. Folglich sind solche Schichtsysteme dem 'reverse engineering' nicht zugänglich. Es werden Beispiele für lateral ausgedehnte, mikrostrukturierte und Laser modifizierte Schichtsysteme auf verschiedenen Ausleseniveaus (menschliches Auge, Barcode-Lesegerät, abbildendes Ellipsometer) vorgestellt, die zur Authentifizierung von Produkten und verwandte Gebiete geeignet sind.
The new promoted ignition combustion test apparatus at BAM matches the requirements of ASTM test method G 124 [ASTM G 124, Standard Test Method for Determining the Combustion Behavior of Metallic Materials in Oxygen-Enriched Atmospheres, 2003] and of EIGA publication, IGC Doc 13/02/E [EIGA Gas Association Document IGC Doc 13/02/E, Oxygen Pipeline Systems, 2003]. The test apparatus is most likely the only one in Europe. The test chamber allows investigations with pure oxygen or oxygen mixtures at pressures up to 500 bar and at temperatures up to 400°C at static or flowing gas conditions. The ignition device consists of an electrical ignition wire and a promoter. IR-sensors, distributed over the whole length of the rod, measure and record the burning temperature and allow measurement of the burn rate. A video system records the experiment for visual characterization of the burning behavior. BAM test results are compared with published data. Results on investigations with coated rods are presented. Ceramic coatings seem to be a solution for the use of certain less compatible metallic materials at higher oxygen pressures.
Two different test apparatuses are used at BAM to evaluate the safety of oxygen components: First, the promoted ignition combustion test according to ASTM G 124 [1] and to EIGA IGC Doc 13/02/E [2], and second, the new metallic disk ignition test that has not been standardized yet. The standard test method ASTM G 124 allows a ranking of metallic materials for use at high pressure oxygen. However, the transfer of those test results to valves and fittings in real-life situations is rather complex. The metallic disk ignition test, developed at BAM, is more practice oriented and uses metallic disks of different thicknesses of the investigated material. A commonly used nonmetallic sealing ring is placed in front of this disk and serves as an igniter. This test array is then exposed to high pressure gaseous oxygen impacts in a standardized pneumatic impact tester according to DIN EN 1797 [3].
Embedding of information on surfaces is state of the art for identification testing in which public, hidden and forensic features are used. In many instances, the legal authentication of a product, a material or a document is required. Among the surface-based encoded labels, bar codes and data matrices are most frequently applied. They are publicly visible. The material itself is irrelevant, only a sufficient optical contrast is required.
However, a strong material dependence of the label can be achieved by means of Fabry-Perot layer stacks. Stack designs are described with regard to all three security levels: public features (e.g. color and tilt effect) perceptible by the human eye, hidden features (e.g. optical response in a given spectral range) detectable by commonly available instruments and forensic features (ellipsometric quantities Ψ and Δ as a function of wavelength λ and angle of incidence AOI) only detectable by sophisticated instruments.
Regarding material-correlated authentication, ellipsometric quantities Ψ and Δ are used as encoded forensic features for the first time. Hence, Fabry-Perot layer stacks as information carriers in combination with imaging ellipsometry as optical read-out system provide all-in-one anti-counterfeiting capabilities.
Standardised conventional adhesion tests are time-consuming single-sample tests. Moreover, except for the pull-off test, all these tests provide only qualitative or semi-quantitative (ranking, respectively measurement of an adhesion-correlated quantity) information on adhesion. Sometimes, adhesion is evaluated even under compressive stress conditions (e.g. cross-cut and scratch test), which itself is a contradiction to adhesive strength as defined in terms of tensile force per area.
For optical coatings it has been shown that the pull-off test in a centrifuge is definitely a promising alternative with respect to the reliable, fast and quantitative determination of adhesive strength in N/mm2. The force-controlled centrifuge test is the only multiple-sample test which provides reliable quantitative information on the adhesive strength in agreement with DIN EN 15870 and DIN EN ISO 4624 on a statistical basis for up to eight samples simultaneously tested under identical testing conditions.
Hybrid optical measurement technique for detection of defects in epitaxially grown 4H-SiC layers
(2022)
Recent developments in power electronics require the use of new wide bandgap compound semiconductor. We demonstrate the use of the ellipsometry and white light interference microscopy to detect defects in epitaxially grown SiC layers on SiC substrates. Such hybrid optical metrology methods can be used to better understand the mechanism of the development of the defects as well as their effects on the material´s optoelectronic properties.
To prevent future alkali-aggregate reaction (AAR) damage, which has occurred frequently in the Germanhighway network in recent years, a new regulation has been drafted. This regulation severely limits the use of alkali-sensitive aggregates by requiring that their suitability be verified by certified inspectors using newly developed AAR concrete tests that involve the external supply of alkali. This has led to a significant limitation in the number of aggregates usable for concrete pavements. A novel AAR avoidance strategy is now being pursued, which aims to enable the use of borderline alkali-sensitive aggregates through the application of an internal water-repellent treatment. The addition of water repellents during concrete production should significantly reduce the ingress of water and external de-icing salts into the concrete pavement, thus reducing the potential for AAR damage.
This paper presents the results of laboratory tests to assess the suitability of this new AAR prevention strategy. Representative, highly AAR-susceptible road paving concrete made with an alkali- sensitive greywacke and various water repellents were used as the basis for these experiments. The tests for concrete suitability included determining the conventional fresh and hardened concrete properties as well as concrete prism tests with external alkaline supply. Building on these results, laser-induced breakdown spectroscopy (LIBS) analyses of de-icing-salt intrusion as well as microscopic examinations for verification of the AAR characteristics were carried out.
The results of the AAR concrete tests with external alkaline supply support the conclusion that, when hydrophobic agents containing a suitable active ingredient are used, the AAR damage process in road paving concrete can be sufficiently prevented.