Analytische Chemie
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Circumventing boundary effects while characterizing epoxy/copper interphases using nanoindentation
(2017)
Characterization of the size and mechanical properties of interphases is essential when designing multicomponent materials. When nanoindentation is used to investigate the size and mechanical properties of an interphase, a common challenge is that the indenter or the stress zone formed around it are often restricted by the reinforcement, making it difficult to distinguish the mechanical property variations caused by the interphase itself from those caused by the boundary effect. In this work, a testing system was developed that allows determining the indent affected zone and accounting for it in the interphase measurements of an epoxy/Cu system. Using finite element analysis, we confirmed the validity of the proposed system. Nanoindentation was used to investigate the Interphase between copper and two different epoxy systems; amine-cured and anhydride-cured. Nanoindentation results showed that a copper layer that is only 10 nm thick still exhibits a constriction effect on the indentations in its vicinity. The amine-cured epoxy did not show any sign of interphase existence using the introduced method. However,
a soft interphase with a thickness of ~1.7 μm was measured on theanhydride-cured epoxy. Furthermore, we show that the proposed system can be used to determine the interphase thickness as well as its relative mechanical properties regardless of the indentation depth.
This system can be further used for investigating other polymer/metal interphases to better understand the factors influencing them, thus helping engineer the interphase size and properties to enhance composite performance.
Applications of X-ray refraction to non-destructive characterization of ceramics and composites
(2017)
X-ray refraction is analogous to visible light deflection by matter, with two main differences: 1- convex objects cause divergence (i.e., the refraction index n is smaller than 1), and 2- deflection angles are very small, from a few seconds to a few minutes of arc (i.e., n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks, and quantify their densities in bulk (light) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation.
We will thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in ceramic science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in diesel particulate filter silicates; 3) fiber de-bonding in metal and polymer matrix composites; 4) micro-cracking of glass-precursor -eucryptite. We will see that the use of X-ray refraction analysis yields quantitative results, also directly usable in available models.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load.
X-ray refraction techniques represent a very promising, yet not so wide-spread, set of X-ray techniques
based on refraction effects. They allow determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with nanometric detectability. While they are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of microstructural features could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography.
Microstructure characterisation of advanced materials via 2D and 3D X-ray refraction techniques
(2018)
3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution in an Al/Al2O3 metal matrix composite during tensile load and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity’s like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography and tomography.
Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise.
This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers.
Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise.
This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers.
The use of composite materials has been steadily growing during the last decades, as well as the requirements on quality, mechanical properties and geometries of the parts. Some processes, like the 3D UV pultrusion process, manufacture parts that are long and thin, whilst having a varying curvature radius along the same part or even no curvature at all. Studying their mechanical properties along the main fiber direction, which is of foremost interest, is not an easy task nor efficient with most nondestructive methods. The use of air-coupled ultrasonics to evaluate the properties of composite materials has been widely proved by several authors, mainly using guided waves that provide information on the orthotropic properties of this kind of materials. Most of this work has focused on analyzing straight plate-like geometries, due to the simplicity to generate desired Lamb modes in the plate and analyze the behavior of guided waves inside the plate. In our contribution, the differences in the propagation of Lamb waves for straight and curved geometry glass fiber reinforced polymers (GFRP) have been analyzed. A GFRP test sample cured with UV light with one straight and one curved area has been evaluated. The responses of the generated Lamb wave modes for the straight and curved geometries have been compared, accounting for variations in the transducer characteristics, e.g. resonance behavior and focusing.
Ultrasonic guided waves (UGW) have been shown to be suitable for non-destructive testing (NDT) and structural health monitoring (SHM) of many engineering structures. Development of a technique based on UGWs requires careful understanding obtained through modelling and analysis of wave propagation and mode-damage interaction due to their dispersion and multimodal character. This presentation will provide insights into the Scaled Boundary Finite Element Method and its applicability for tackling wave propagation problems. Features and limitations of the SBFEM will be presented on an example of a multi-layered plate structure consisting of isotropic and anisotropic materials bonded together. You will be guided through the process of picking up the wave modes for your application. Starting from the calculation of dispersion curves and mode shapes to the analysis of wave propagation and mode-damage interaction. The main highlight of the presentation lies in the ability to detect damage in a certain layer depending on the mode used. The resulting deeper understanding of the wave propagation in multi-layered structures is the key to further developments of NDT and SHM for engineering structures consisting of multiple layers.
Akustische Verfahren eignen sich hervorragend zur Bestimmung der Werkstoffeigenschaften. Die Verfügbarkeit derartiger Verfahren ist vor allem für Kunststoffe wichtig, da deren Eigenschaften stark abhängig vom jeweiligen Herstellungsprozess und vom Alterungszustand sind. Exakte und vollständige Werte sind daher in Datenbanken oder von Herstellern nur begrenzt zu finden. Insbesondere die Entwicklung von Methoden zur Charakterisierung faserverstärkter Kunststoffe (FKV) ist nach wie vor Gegenstand der Forschung. Hier müssen anisotropiebedingt mehrere Kennwerte bestimmt werden. Da FKV zumeist als dünnwandige Bauteile zum Einsatz kommen, können die Werkstoffparameter aus den Dispersionseigenschaften der Lamb-Wellen, die sich in diesen Strukturen ausbreiten, abgeleitet werden. Dazu ist eine räumliche Abtastung des sich ausbreitenden Schallfelds erforderlich.
In der vorliegenden Untersuchung wird dieser Ansatz für die relativ neue Werkstoffklasse der faserverstärkten Thermoplaste angewendet. Diese zeichnet ein ausgeprägtes Dämpfungsverhalten und eine Anisotropie der Materialparameter aus. Dazu wurde das Schallfeld im Ultraschallbereich mit einem Laser-Doppler-Vibrometers vermessen. Rechnerisch bestimmte Dispersionskurven wurden dann an die gemessenen Werte angepasst, womit die richtungsabhängigen Materialparameter bestimmt werden konnten.
Im Vortrag wird das Messverfahren vorgestellt und auf spezielle Probleme, die sich z.B. aus dem Dämpfungsverhalten des Werkstoffs ergeben, eingegangen. Ausgewählte gemessene Werte werden mit den Ergebnissen von Referenzverfahren verglichen.