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- ALD Haftvermittler (1)
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- Imaging Ellipsometrie (1)
- Imaging ellipsometry(IE) (1)
- Instrumented Indentation (IIT) (1)
- Instrumented Indentation Testing (IIT) (1)
- Instrumented indentation testing (1)
- Instrumentierte Eindringprüfung (IIT) (1)
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- Multiple-sample bonding (MSB) (1)
- Multiple-sample handling (MSH) (1)
- Niedrigenergie-Polymeren (1)
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- PVD-coatings (1)
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- Particles as add-on features (1)
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- Particulate distributions (1)
- Physical vapour deposition (PVD) (1)
- Plasma activation (1)
- Plasma-assisted ALD modification (1)
- Prüfgeschwindigkeiten (1)
- Prüfverfahren (1)
- Pull-off test (1)
- Quality Control (1)
- Reference procedures (1)
- Ringversuch Ellipsometrie (1)
- Schichttechnik (1)
- Selbstkalibrierung (1)
- Spectroscopic ellipsometry (1)
- Spektrale Ellipsometrie (SE) (1)
- Statistischen Untersuchung (1)
- Structural health monitoring (1)
- Structural health monitoring (SHM) (1)
- Stumpfklebungen (1)
- Surface plasmon resonance (SPR), (1)
- Surface plasmon resonance enhanced ellipsometry (SPREE) (1)
- TCO (1)
- Tensile Stress (1)
- Tensile strength of coatings (1)
- Tensile strength of laminates (1)
- Topographie (1)
- Unintended particle generation (1)
- Verunreinigungen (1)
- Weißlichtinterferenzmikroskopie (1)
- Weißlichtinterferenzmikroskopie (WLIM, 3D) (1)
- White light interference microscopy (1)
- Zentrifugentechologie (1)
Organisationseinheit der BAM
- 6 Materialchemie (26)
- 6.7 Materialsynthese und Design (25)
- 6.1 Oberflächen- und Dünnschichtanalyse (3)
- 6.2 Material- und Oberflächentechnologien (3)
- 8 Zerstörungsfreie Prüfung (3)
- 8.6 Faseroptische Sensorik (3)
- 8.1 Sensorik, mess- und prüftechnische Verfahren (2)
- 6.6 Physik und chemische Analytik der Polymere (1)
Eingeladener Vortrag
- nein (39)
The lack of on-line validation procedures for structure-embedded fiber-optical strain sensors, in particular fiber-Bragg-gratings (FBG), resulted in limited applications in structural health monitoring (SHM). Degradation under service conditions and ageing as a result of climatic influences or delamination under load were unsolved Validation issues. This could be overcome by means of an auto-diagnosis procedure based on FBG-sensors coated by electrochemical deposition (ECD) with a magnetostrictive NiFe-coating on top of an adhesive Cu/Cr adhesive layer deposited by physical vapour deposition (PVD) around the FBG strain sensor. This allows at any time under Service a validation of sensor functionality, stability, and reliability. For this purpose, a magnetic strain-proportional reference field is introduced. The optical read-out is realized by the measurement of the Bragg-wavelength shift.
The ratio of resulting strain and exciting magnetic reference field should be constant given that the sensor is in proper function.
In principle, the magnetostrictive coating around the FBG should also work as on-line magnetic field sensor and other applications in material science. One of these applications is the in-situ monitoring of ECD processes as the deposition of the ECD NiFe-layer on the FBG revealed. Challenges are the monitoring of temperature, deposition
stages/thickness, and resulting mechanical stress under given plating conditions. Monitoring problems can be solved by applying a pre-coated FBG to the electrolytic process as the shift of the Bragg wavelength is affected by both the temperature of the electrolyte near the substrate and the stress formation in the growing layer. The experimental FBG set-up and the quantitative determination of temperature- and stress-related strain are described for a nickeliron
electrolyte. The in-situ measurement of Bragg wavelength shifts of a pre-coated FBG during electrochemical deposition allows a detailed analysis of stress states due to changes in the growth morphology of the layer. The separation of mechanical and thermal contributions to this shift provides information on the individual Deposition processes in terms of a process fingerprint.
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.
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.
Der Vortrag widmet sich der „Zentrifugentechnologie zur statistischen Untersuchung von Stumpfklebungen“ und beschreibt drei wesentlich verschiedene Realsysteme (Fügefläche 1/Klebstoff/ Fügefläche 2), um die Statistik ZPM (wiederholte Ein-Proben-Prüfung) vs. CAT (Mehr-Proben-Prüfung) zu vergleichen. Dazu wurden drei unterschiedliche Klebstoff-klassen mit typischen Fügeteilmaterialkombinationen ausgewählt und in einem Vorversuch mit jeweils 3 unterschiedlichen Prüfgeschwindigkeiten sowohl im Weg-geregelten als auch Kraft-geregelten Mode beansprucht. Die Ergebnisse ZPM vs. CAT und Kraft- vs. Weg-Regelung des Vorversuches zeigten keinerlei Unterschiede auf. Im Ergebnis wurde ein Ringversuch im Kraft-geregelten Mode (6xZPM vs. 8xCAT) für ein Referenzsystem durchgeführt, der nachwies, dass die CAT-Technologie statistisch relevante Prüfergebnisse zur Klebfestigkeit bereitstellt. Es zeigte sich, dass für zwei ZPM-Teilnehmer im Vertrauensbereich 99% statistisch signifikant etwas kleinere Werte der Klebfestigkeit bestimmt wurden, was auf geringfügige Abweichungen von der axialen Ausrichtung des eingespannten Prüflings bei der Ein-Proben-ZPM-Zugprüfung zurückgeführt wird.
Mechanische, topometrische und optische Charakterisierung von Schichten mit Stand der Normung
(2019)
Der Vortrag „MECHANISCHE, TOPOMETRISCHE UND OPTISCHE CHARAKTERISIERUNG VON SCHICHTEN MIT STAND DER NORMUNG“ widmet sich unterschiedlichen Beschichtungssystemen und deren mechanischer, topometrischer und optischer Charakterisierung. Über die entsprechenden aktuellen Normen wird informiert. Es betrifft Verfahren wie die Instrumentierte Eindringprüfung (IIT), Centrifugal Adhesion Testing, Weißlichtinterferenzmikroskopie, Tastschnittverfahren und Ellipsometrie (SE).
Der Vortrag widmet sich der „ CAT-TECHNOLOGIE ZUR BESTIMMUNG DER KLEBFESTIGKEIT“ und beschreibt die Punkte „Motivation –CAT-Technologie (Centrifugal Adhesion Testing), Klebfestigkeit ( Materialscreening verschiedener Werkstoffklassen, Klebstoffscreening fürV2A gegenV2A als Referenz, Klebstoffscreening für Niedrigenergie-Polymere und Oberfächenmodifizierung von Niedrigenergie-Polymeren) und Verbundfestigkeit (“Stirnabzug vs. Zug-Scher-Prüfung an CFK) im Einzelnen.
Der Vortrag widmet sich der „CAT-TECHNOLOGIE ZUR BESTIMMUNG DER HAFTFESTIGKEIT DÜNNER SCHICHTEN“ und beschreibt die Punkte „Motivation –CAT-Technologie“ (CAT: Centrifugal Adhesion Testing) und die „Haftfestigkeit von Schichten“, (Ag-Schichten auf N-BK7 Glas, Cr- und Al-Schichten auf Borofloat 33 Glas, Au-Schichten auf N-BK7 Glas und SiO2-Schichten auf CR39 Polymer) im Einzelnen.
Up until several years ago, tensile and compressive tests have been exclusively carried out as single-sample tests within a tensile, hardness or universal testing machine. The availability of centrifuge technology changed this situation in 2013 in several ways because centrifugal force is used as testing force within a rotational reference frame.
Firstly, multiple-sample strength testing became feasible for both tensile load condi-tions, e.g. determination of composite, bonding or adhesive strength, and compressive load conditions, e.g. hardness, compressibility and compactibility. Secondly, there is no need for a two-sided sample clamping and double-cardanic suspensions as samples are simply inserted using a one-sided sample support. Thirdly, shear forces can be avoided by means of guiding sleeves which steer test stamps acting as mass bodies for either tensile or compressive testing. Fourthly, up to eight samples can be tested under identical conditions within a very short period of time, typically within 15 minutes including sample loading and unloading. Hence, either a reliable statistics (of identical samples) or a ranking (of different samples) can be derived from one test run.
The bench-top test system is described in detail and demonstrated that centrifugal force acts as testing force in an appropriate way because Euler and Coriolis force do not affect the testing results. Examples for both tensile strength testing, i.e. bonding strength of adhesives-bonded joints and adhesive strength of coatings, and compres-sive strength testing, i.e. Vickers-, Brinell- and ball indentation hardness and deter-mination of spring constants, are presented, discussed and compared with conven-tional tests within tensile, hardness or universal testing machines.
At present, a maximum testing force of 6.5 kN can be realized which results at test stamp diameters of 5 mm, 7 mm, and 10 mm in tensile or compressive stress values of 80 MPa, 160 MPa, and 320 MPa. For tensile strength, this is already beyond bonding strength of cold- and warm-curing adhesives. Moreover, centrifuge technology is compliant to standards such as EN 15870, EN ISO 4624, EN ISO 6506/6507 and VDI/VDE 2616. Programmable test cycles allow both short-term stress and log-term fatigue tests. Based on a variety of examples of surface and bonding technology, applications in both fields R&D and QC are presented. Meanwhile, centrifuge technology is also accredited according to DIN EN ISO/IEC 17025.
Der Vortrag gibt den aktuellen Stand der Normung im Bereich der Oberflächentechnik insbesondere der Oberflächenanalytik und der Oberflächenmess- und -prüftechnik wider. Vorgestellt wird der Status technischer Berichte, Normenentwürfe und Normen u.a. zur Bewertung von Auflösung und Schärfe mit strahlbasierten Methoden im Nanometer- und Mikrometerbereich, zur Messung von Schichtdicken und Nanopartikeln in kritischen Dimensionen einschließlich Größen- und Formverteilungen mittels REM, zur Messung der Schichtdicke von Nanomaterialien und zur Klassifizierung von Kohlenstoffschichten mittels Ellipsometrie, zur Standardisierung der Ellipsometrie, zur Kalibrierung von Konfokalmikros-kopen für die Formmessung, zur linear elastisch dynamischen instrumentierten Eindringprüfung, zur Messung der flächenbezogenen Masse mittels AAS und ICP, zur Schichtpotentialmessung von Mehrfach-Nickelschichten, zur Schichtdicken und Flächen-widerstandsbestimmung sowie zur Bestimmung der Schichthaftung mittels Zentrifugentechnologie.
Mit der Zentrifugentechnologie ist seit einigen Jahren ein neuartiges Mehr-Proben-Prüf-verfahren auf dem Markt etabliert, welches die klassische Zugprüfung in den Trommelrotor einer Tischzentrifuge überträgt. In der Beanspruchung auf Zug ist die Prüfung der Verbundfestigkeit mittels CAT-Technologie (centrifugal adhesion testing) an der BAM seit 2017 nach DIN EN ISO/IEC 17025 akkreditiert, wobei die Verbundfestigkeit von Klebungen direkt bestimmt wird und in Abhängigkeit von den Versagensformen Rückschlüsse auf die Klebfestigkeit von Klebstoffen/Klebebändern oder die Haftfestigkeit von Beschichtungen gezogen werden können.
The application of PVD-coatings ranges from mechanical engineering, i.e. thicker tribological coatings, to precision optics, i.e. thinner optical coatings. For physical vapor deposition (PVD) technologies such as evaporation, sputtering, ion beam assisted/driven deposition, vacuum is a prerequisite for two reasons: at first process-related ones (evaporation source, plasma discharge, and mean free path) and at second coating-related ones (pure, perfect, and dense films). Usually, the goal is a homogenous coating of defined stoichiometry and micro-structure without any imperfection.
However, the implementation of micro- or nano-particles may occur accidentally or delibe-rately. Independent of the particle origin, there are two fundamental rules regarding coating functionality: at first, the larger the particle diameter to coating thickness ratio the more affected the functionality of the coating, and at second, the larger the material contrast in terms of the functional feature of interest the more affected the coating performance. Hence, embedded particles have to be avoided for the majority of thin films by all means. The unintended implementation of particles usually results in a malfunction of the coating from the beginning or is at least considered as a weak point of the coating creating a time-dependent defect under service conditions. The intended implementation of particles on surfaces and in coatings may create add-on features, topographic ones and functional ones, however, the facts mentioned hold true.
Examples of particle-initiated coating defects are demonstrated in dependence on the origin and the field of application. Strategies for deliberate attachment/embedding of particles on surfaces/in coatings are discussed regarding process compatibility and coating integrity. For industrial applications, both the validation of process compatibility of particle injection and the plasma resistance of particles under vacuum and plasma conditions have to be confirmed. Further points of interest are the homogeneity of particle distribution and the avoidance of particle agglomeration which is still a crucial point for dry dispersed particles. So far, technical applications are limited to PVD hybrid coatings, plasma dispersion coatings are still a challenge except for applications where homogeneity is not required as in case of product authentication.
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 paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures.
The talk addresses the STANDARDIZATION OF ELLIPSOMETRY and the following points are discussed in more detail: historical background of ellipsometry, history of International Conferences on Ellipsometry, Workshops Ellipsometry in Germany and Europe, information on German/European Working Group Ellipsometry, technical/industrial importance of ellipsometry, applications on non-ideal material systems and standardization activities on ellipsometry.
Transparent conductive oxide (TCO) films are a vital part of a large part of modern technology. The production of TCO materials has sparked much development in plasma coating technology. Quality control measurements of these layers are therefore important in many fields of optics and electronics such as high efficiency thin film photovoltaics. In this presentation, we report on optical measurements of ZnSnOx layers generated by DC/RF magnetron plasma co-sputtering. By changing the respective power on two different targets, the overall power, the gas composition and post-treatment, the properties of this type of layers can be varied in a number of parameters. The optical, electrical, and chemical properties of TCO layers are the technically most important properties together with the layer thickness. The dielectric function of layers is accessible by means of spectroscopic ellipsometry, which also yields the very important value for the layer thickness at the same time. It would be a significant step forward in quality control to use this non-destructive method also as a fast test for electrical properties. Therefore, we report on the optical properties connected to the production parameters, and also on our preliminary results connecting the optical dielectric function (in the visible and near infrared) to the electrical conductivity of the layers. We discuss the effect of deposition parameters on the optical properties of the layers and present an approach for correlating optical and electrical properties. Further, we discuss the question of accuracy of optical properties gained from model-fit-based optical methods and the use of different parameterised models for the dielectric function to achieve this.
Multi-functional coatings are a key requirement for surface engineering. General demands are adhesion and long-term stability under service conditions. The modification of surfaces by means of PVD-, ECD- or hybrid processes allows an add-on functionalization of surfaces by a huge diversity of materials with both lateral and vertical micro-/nano-designs. This fact is a prerequisite for micro- and sensor-systems in lab-on-chip and sensor-on-chip technology. Two layer-based sensor principles are presented, i.e. surface plasmon resonance enhanced spectroscopic ellipsometry (SPREE) for detection of hazardous gases and magneto-optical sensors on smart-coated fiber Bragg gratings (FBG) for structural health monitoring (SHM).
The interdependence of substrate features, coating properties, and layer design is discussed firstly for gas sensitivity and selectivity of SPREE-sensors and secondly for sensitivity and selectivity of magneto-strictive coatings to mechanical strain or external magnetic fields resulting in an optical displacement of the Bragg wavelength of FBG-sensors. Moreover, generic features such long-term stability, crucial process-related fabrication conditions, and effects of operational and environmental parameters are discussed with respect to the sensor performance. It has been shown that appropriate layer design and adapted selection of layer materials (SnOx/Au, Fe/Ni:SnOx/Au; Ni/NiFe-Cu-Cr) result in improved sensor parameters and may enable new sensor applications.
Der Vortrag widmet sich der „ELLIPSOMETRISCHE KLASSIFIZIERUNG VON KOHLENSTOFFSCHICHTEN“ und beschreibt die Punkte: 1. Anwendungen Kohlenstoffschichten–Carbon–based films (DLC) aus dem Vortrag N. Ohtakeet. al. (ISO TC 107, Tokyo 2017),2. Präparation der Kohlenstoffschichten für ISO TC 107 Ringversuch aus Vortrag M. Hiratsuka et. al. (ISO TC 107, Tokyo 2017), 3. Ellipsometrische Charakterisierung von Kohlenstoffschichten, Ergebnisse des Ringversuchs (ISO TC 107, Tokyo 2017) Vortrag Beck et. al. und 4.Deutsche Normungsaktivitäten national/international zur Ellipsometrie DIN NA 062-01-061 (DIN 50989-1)/TC 107 (PWI DE)“ im Einzelnen.