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Chapter 6: Case studies
(2023)
Nanotechnologien werden gegenwärtig als leistungsfähige Oberflächentechniken in erheblichem Umfange industriell genutzt. Dabei spielen dünne Schichten und deren Kenndaten eine wesentliche Rolle, z.B. als Röntgenspiegel oder optische und magnetooptische Datenträger. Die Schichtdicke zählt hierbei zu den technologisch wichtigen Parametern. Abgeleitet von Anwenderinteressen, werden für die Röntgenreflektometrie (XRR bzw. GIXR), Elektronenstrahl-Mikroanalyse (EPMA) und Röntgenfluoreszenzanalyse (XRF) einerseits und die Ellipsometrie andererseits zugeschnittene Schichtdickenmaßverkörperungen (SDM) entwickelt, gefertigt und untersucht. Das Ziel ist die Bereitstellung praxistauglicher, kalibrierter SDM, im weiteren Schichtdickennormale (SDN) genannt. SDN sind Maßverkörperungen, für die der Schichtdickenwert mit einer definierten Messunsicherheit bekannt und auf ein metrologisch anerkanntes Längennormal zurückgeführt ist. Berichtet wird über die Herstellung und messtechnische Charakterisierung der beiden spezifischen Varianten von Maßverkörperungen.
Die Magnesiumlegierung Mg-Cal besitzt als potentielles bioabsorbierbares Implantatmaterial die Möglichkeit, vollständig vom menschlichen Körper absorbiert zu werden. Die mechanischen Kennwerte dieser Legierung liegen im Bereich des menschlichen Knochens und beide Legierungselemente (Mg, Ca) sind essentielle Spurenelemente im menschlichen Organismus.
Der limitierende Faktor für den Einsatz ist die hohe Degradationsrate dieser Legierung. Um die Degradationsgeschwindigkeit zu verringern, wurden zwei Beschichtungssysteme auf Grundlage der Plasmachemischen Oxidation (PCO) und organischer Beschichtung erzeugt und untersucht. Das Korrosionsverhalten dieser Schichtsysteme wurde dabei mit dem Elektrochemischen Rauschen analysiert. Zusätzlich wurde der Einfluss von Wasserstoffentwicklung und eines ansteigenden pHWert auf die Zelltoxizität untersucht. Die Ergebnisse zeigen, dass eine Kombination von beiden Schichtsystemen zu einem viel versprechenden Degradationsverhalten führt.
High-accuracy film thickness measurements in the range below 100 nm can be made by various complex methods like spectral ellipsometry (SE), scanning force microscopy (SFM), grazing incidence X-ray reflectometry (GIXR), or X-ray fluorescence analysis (XRF). The measurement results achieved with these methods are based on different interactions between the film and the probe. A key question in nanotechnology is how to achieve consistent results on a level of uncertainty below one nanometre with different techniques.
Two different types of thickness standards are realised. Metal film standards for X-ray techniques in the thickness range 10 to 50 nm are calibrated by GIXR with monochromatised synchrotron radiation of 8048 eV. The results obtained at four different facilities show excellent agreement. SiO2 on Si standards for SE and SFM in the thickness range 6 to 1000 nm are calibrated by GIXR with monochromatised synchrotron radiation of 1841 eV and with a metrological SFM. Consistent results within the combined uncertainties are obtained with the two methods. Surfaces and interfaces of both types of standards are additionally investigated by transmission electron microscopy (TEM).
The main problem limiting the application of magnesium alloys as biodegradable implant material is its high degradation rate. In order to slow down the corrosion rate an extrusion process and specific coating systems based on plasma-chemical oxidation (PCO) and organic dip coating with poly(ʟ-lactid-co-caprolacton) (PLLC) were applied on Mg–1Ca magnesium alloy. The additional PLLC coating is used to delay the start of substrate corrosion, while the purpose of the PCO coating is to decrease the substrate corrosion rate. The corrosion behaviour was investigated in synthetic body fluid (SBF) through measurement of the hydrogen evolution rate in long term tests and polarisation and electrochemical noise measurements in short term tests. The results showed significant differences between the cast and extruded alloys and a decrease of the corrosion rate due to corrosion product formation. The combination of both coating systems resulted in a significant delay of metal substrate corrosion and all coating systems showed good correlation between short and long term tests. The combination of the three investigation methods provides the possibility to gain more information about the degradation behaviour and break down of protective coatings.
Hands-off linear interaction energy approach to binding mode and affinity estimation of estrogens
(2013)
With this work we target the development of a predictictive model for the identification of small molecules which bind to the estrogen receptor alpha and, thus, may act as endocrine disruptors. We propose a combined thermodynamic approach for the estimation of preferential binding modes along with corresponding free energy differences using a linear interaction energy (LIE) ansatz. The LIE model is extended by a Monte Carlo approach for the computation of conformational entropies as recently developed by our group. Incorporating the entropy contribution substantially increased the correlation with experimental affinity values. Both squared coefficients for the fitted data as well as the more meaningful leave-one-out cross-validation of predicted energies were elevated up to rFit2 = 0.87 and qLOO2 = 0.82, respectively. All calculations have been performed on a set of 31 highly diverse ligands regarding their structural properties and affinities to the estrogen receptor alpha. Comparison of predicted ligand orientations with crystallographic data retrieved from the Protein database pdb.org revealed remarkable binding mode predictions.
The presence of elongation, streak and blurring artifacts in tomograms recorded under a missing wedge of rotation angles presents a major challenge for the quantitative analysis of tomographic image data. We show that the missing wedge artifacts of standard reconstruction algorithms may be reduced by the innovative reconstruction technique DIRECTT. For the comparison of missing wedge artifacts we apply techniques from spatial statistics, which have been specifically designed to investigate the shape of phase boundaries in tomograms.
Incomplete tomographic data sets such as limited view (missing wedge) data represent a well-known challenge
for reconstruction algorithms, since they unavoidably lead to substantial image artefacts. Such data sets may
occur in industrial computed tomography of limited access (e.g. extended components, fixed objects), directional
opacity, limited sample life time or laminographic set-up. We present strategies to effectively suppress the
typical elongation artefacts (e.g. lemon-like deformed pores) by our iterative algorithm DIRECTT which offers
the opportunity to vary the versatile reconstruction parameters within each cycle. Those strategies are applied to
experimental data obtained from metallic foams as well as model simulations. Comparison is drawn to state-ofthe-
art techniques (filtered backprojection and algebraic techniques). Further reference is made to reconstructions
of complete data sets serving as gold standards. For quantitative assessment of the reconstruction
quality adapted techniques based on spatial statistics are introduced.
We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets.
Till now application of printed magnetoelectronics is hindered by lack of large area exchange coupled metallic multilayers required to produce printable magneto-sensory inks. Large-scale roll-to-roll (R2R) fabrication process is an attractive approach owing to its capabilities for high volume, high throughput, and large area manufacturing. Precise and high performance R2R sputtering technology is developed to fabricate large area giant magnetoresistive (GMR) thin-films stacks that contain 30 metallic bilayers prepared by continuous R2R sputtering of Co and Cu sequential on a hundred meters long polyethylene terephthalate (PET) web. The R2R sputtered Co/Cu multilayer on a 0.2 × 100 m2 PET web exhibits a GMR ratio of ≈40% achieving the largest area exchange coupled room temperature magneto-sensitive system demonstrated to date. The prepared GMR thin-film is converted to magnetosensitive ink that enables printing of magnetic sensors with high performance in a cost-efficient way, which promotes integration with printed electronics. An average GMR ratio of ≈18% is obtained for 370 printed magnetic sensors. The realized precise R2R sputtering approach can also be extended to a wide range of hybrid thin-film material systems opening up a path for new functional inks applied with printing technologies.
The explosion characteristics of anthracite coal dust with/without small amount of CH4 (1.14 vol %) were investigated by using a 20 L spherical explosion apparatus with an emphasis on the roles of oxygen mole fraction and inert gas. Two methods based on overpressure and combustion duration time were used to determine the minimum explosion concentration (MEC) or the lower explosion limit (LEL) of the pure anthracite coal dust and the hybrid coal-methane mixtures, respectively. The experiment results showed that increasing oxygen mole fraction increases the explosion risk of coal dust: with increasing oxygen mole fraction, the explosion pressure (Pex) and the rate of explosion pressure rise ((dp/dt)ex)) increase, while MEC decreases. The explosion risk of anthracite dust was found to be lower after replacing N2 with CO2, suggesting that CO2 has a better inhibition effect on explosion mainly due to its higher specific heat. However, the addition of 1.14% CH4 moderates the inhibition effect of CO2 and the promotion effect of O2 on anthracite dust explosion for some extent, increasing explosion severity and reducing the MEC of anthracite dust. For hybrid anthracite/CH4 mixture explosions, Barknecht’s curve was found to be more accurate and conservative than Chatelier’s line, but neither are sufficient from the safety considerations. The experimental results provide a certain help for the explosion prevention and suppression in carbonaceous dust industries.
Typische 'Missing Wedge'(MW)-Artefakte in Rekonstruktionen der Computertomografie können mit dem iterativen DIRECTT-Algorithmus (Direkte iterative Rekonstruktion computertomografischer Trajektorien) unterdrückt werden. Die durch fehlende Projektionswinkel bedingten MW-Restriktionen betreffen bisher nur Sonderapplikationen der Röntgen- und Neutronentomografie, müssen in der Nanometer auflösenden Elektronentomografie jedoch als Standard akzeptiert werden. Die MW-Artefakte werden besonders effektiv mit einer spezifischen DIRECTT-Prozedur partiell diskreter Zwischenlösungen beseitigt. Für die Beurteilung der Abbildungsqualität werden Rekonstruktionen von vollständigen und unvollständigen Mess- und Modell-Datensätzen erzeugt und mit Ergebnissen anderer Algorithmen (gefilterte Rückprojektion (FBP) und ART-Methoden) verglichen. Die Fourier-Transformierten der Rekonstruktionen demonstrieren die erfolgreiche Ergänzung der fehlenden Information im MW-Bereich. Die quantitative Bewertung der lokalen Rekonstruktionsqualität mit Methoden der räumlichen Statistik ergibt auch für unterschiedliche Signal-Rausch-Verhältnisse signifikante Vorteile gegenüber FBP und ART.