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- Adjustment calculation (2)
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Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of lattice structures. These lattice structures shall be implemented in various industrial applications (e.g. gas turbines) for reasons of material savings or cooling
channels. However, internal defects, residual stress, and structural deviations from the nominal geometry are unavoidable.
In this work, the structural integrity of lattice structures manufactured by means of L-PBF was non-destructively investigated on a multiscale approach.
A workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established.
Synchrotron computed tomography (CT) was used to correlate the packing
density with the particle size and particle shape. It was also observed that at least about 50% of the powder porosity was released during production of the struts.
Struts are the component of lattice structures and were investigated by means of laboratory CT. The focus was on the influence of the build angle on part porosity and surface quality. The surface topography analysis was advanced by the quantitative characterisation of re-entrant surface features. This characterisation was compared with conventional surface parameters showing their complementary
information, but also the need for AM specific surface parameters.
The mechanical behaviour of the lattice structure was investigated with in-situ CT under compression and successive digital volume correlation (DVC). The Deformation was found to be knot-dominated, and therefore the lattice folds unit cell layer wise.
The residual stress was determined experimentally for the first time in such lattice structures. Neutron diffraction was used for the non-destructive 3D stress investigation. The principal stress directions and values were determined in dependence of the number of measured directions. While a significant uni-axial stress state was found in the strut, a more hydrostatic stress state was found in the knot. In both cases, strut and knot, seven directions were at least needed to
find reliable principal stress directions.
Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis
(2019)
The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis.
First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface.
Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios.
Zusammenfassung
Die vorliegende Arbeit befasst sich mit zwei zentralen Aspekten der High-Resolution-Continuum-Source-Molekülabsorptionsspektrometrie mit Graphitrohrtechnik (HR-CS-GFMAS), einer Analysetechnik für elementare Spurenanalyse.
Der erste Teil der Arbeit umfasst eine mechanistische Studie zur Molekülbildung auf Graphitoberflächen. Dies ist ein wichtiger Schritt, um analytische Signale zu entdecken. Dazu wurde die Molekülbildung von CaF analysiert, welches für die indirekte, analytische Bestimmung von Fluor in HR-CS-GFMAS genutzt wird. Die CaF Bildung wurde mittels einer Beschichtung aus Zirconium katalysiert und deren Struktur analysiert. Die Kinetik dieser Reaktion wurde durch Beobachtung des jeweiligen Molekülspektrums bei verschiedenen Atomisierungstemperaturen beobachtet. Ein Arrheniusplot zeigte für Fluor (n = 1) eine Reaktion Pseudo-erster Ordnung. Ein Übergangszustand wurde über die mit Zirconium überzogene Grafitoberfläche isoliert und seine Struktur mittels spektroskopischer Methoden Energiedispersive Rasterelektronenmikroskopie / Röntgenspektroskopie (REM-EDX), Röntgenphoto¬elektronenspektroskopie (XPS), Röntgenabsorptionsspektroskopie (XAS) und Raman Spektroskopie untersucht. Auf Grundlage dieser Ergebnisse wird ein Mechanismus vorgeschlagen, bei dem ZrO2 als heterogener Katalysator fungiert; in Folge einer Pyrolysestufe wird ein Übergangszustand des ZrO(OCaF) aktiviert, welcher bei höheren Temperaturen CaF(g) an der Zirconium-Graphitoberfläche freisetzt.
Im zweiten Teil der Arbeit werden Analysemethoden entwickelt, in dem HR-CS-MAS als Detektor für Nichtmetalle und Isotopanalyse angewandt wird. Hierfür wurde organisch gebundenes Chlor im Wasser bestimmt, der Fluorgehalt in Pflegeprodukten mit perfluorierten Inhaltsstoffen quantifiziert und der Schwefelgehalt in Erdöl untersucht. Weiterhin ermöglicht die hohe Auflösung der Messgeräte eine präzise Bestimmung der Isotopenverschiebung einiger untersuchter Molekülspektren. Daher wurden die Molekülspektren angereicherter Bor- und Magnesiumisotope untersucht. Auf diese Weise wurde das Potential von HR-CS-MAS für die akkurate und präzise Bestimmung von Isotop-Mengenverhältnissen nachgewiesen.
Free-living and (ecto)-mycorrhizal fungi enhance rock weathering. In their roles as mineral weathering agents and mutualistic partners of phototrophs, fungi supply primary producers like plants and phototrophic microorganisms with mineral-derived nutrients. The exact mechanisms behind fungus-induced mineral weathering processes are however not well understood. Progress can be achieved here by reproducible experimental simulations of the natural processes, using well-characterised model organisms and minerals.
In this study, the weathering-affecting, rock-inhabiting fungus, Knufia petricola A95 and the Fe-bearing olivine (Fe0.2Mg1.8SiO4) were selected to investigate fungi-induced effects on mineral dissolution. The availability of a melanin-deficient mutant (ΔKppks) of K. petricola A95, that produced more extracellular polymeric substances (EPS) than the wild type (WT), enabled comparative studies of the role of melanin and EPS in weathering processes.
Three experimental systems, which generate long-term microbiological stability, were developed to study the impact of the WT and ΔKppks on olivine weathering: (1) batch and (2) mixed flow dissolution experiments, and (3) biofilm cultivation experiments. In addition, state-of-the-art analytical techniques were used to monitor changes in the growth medium, as well as of the mineral surface and biofilm-mineral interface.
Inductively coupled plasma optical emission spectrometry (ICP-OES) analysis of the Mg, Si and Fe concentrations in the reacted growth medium was used to quantify olivine dissolution. In abiotic controls, Mg and Si dissolved congruently, while Fe precipitated. The measured olivine dissolution rates at pH 6 were two orders of magnitude lower than previously reported, but similar at acidic pH. X-ray photoelectron spectroscopy (XPS) analyses of the olivine surface confirmed the presence of Fe (oxyhydr)oxide precipitates. Transmission electron microscopy (TEM) imaging of an abiotically reacted polished olivine section from the long-term cultivation experiment showed the presence of an amorphous layer enriched in Fe. All these observations indicate that the precipitation of Fe (oxyhydr)oxides on the olivine surface inhibits olivine dissolution.
Both tested rock-inhabiting fungal strains affect Fe precipitation as well as olivine dissolution. Evaluation of the WT and ΔKppks revealed that the WT formed less biomass but could take up higher amounts of metals (e.g. Fe) and was more efficient in its attachment to olivine. The WT and ΔKppks enhanced olivine dissolution as demonstrated by higher Mg and Si concentration in the reacted growth medium. They furthermore prevented Fe precipitation by binding Fe and retaining it in solution, thereby allowing olivine dissolution to proceed. The WT cells that were attached to the olivine surface were particularly efficient at inhibiting Fe precipitation. By binding Fe directly at the olivine surface, the WT cells removed the inhibition of olivine dissolution almost completely. TEM analysis of polished olivine sections, colonised by a fungal biofilm for seven months, supported this hypothesis. After long-term fungus-olivine interaction, the Fe-enriched, amorphous layer did not develop, and the olivine surface was stronger etched compared to the abiotic control.
To study the effect of mutualism on mineral weathering, K. petricola was grown with the cyanobacterium, Nostoc punctiforme ATCC 29133. Both partners showed an enhanced growth and formed a stratified biofilm which attached more strongly to olivine. Nevertheless, the olivine dissolution rate of the fungus-cyanobacterium consortium was moderate.
Rock weathering simulation systems developed here are promising research instruments. The experimental conditions allow for the alteration of the studied mineral surface, while the clear definition of these conditions delivers a stable growth of microorganisms. The latter makes these systems universally applicable, especially in combination with integrative multidisciplinary analytics. Processes underlying environmental and biological effects on rock weathering, metal corrosion, plastic degradation, or the deterioration of any other substrate can be studied reproducibly and over a long period of time. The chemical and biological complexity of these simulation systems mimics natural rock weathering processes. The mineral dissolution rates generated in this study are therefore relevant to natural ecosystems.
Concrete is a complex material and can be modeled on various spatial and temporal scales. While simulations on coarse scales are practical for engineering applications, a deeper understanding of the material is gained on finer scales. This is at the cost of an increased numerical effort that can be reduced by the three methods developed and used in this work, each corresponding to one publication.
The coarse spatial scale is related to fully homogenized models. The material is described in a phenomenological approach and the numerous parameters sometimes lack a physical meaning. Resolving the three-phase mesoscopic structure consisting of aggregates, the mortar matrix and the interfaces between them allow to describe similar effects with simpler models.
The simulation of the structural response for impact scenarios strongly requires an accurate simulation of both the impact event as well as the subsequent wave propagation. The numerical modeling of the impact event is intrinsically ill-posed due to the instantaneous changes of velocities in the contact area, leading to unbounded accelerations for decreasing time steps which causes oscillations in the contact stresses. These oscillations then propagate into the bulk material. Using a rate dependent material model, like concrete, they might lead to significant errors and a wrong prediction of the structural response. A regularization is thus required to avoid oscillations in the contact stresses. Another issue is related to the numerical computation of the contact conditions. In impact simulations, the nonlinear contact computation needs to be evaluated in every time step. A segmentation technique of the contact area is accurate but time consuming and may result in a bottleneck for the simulation and implementation, especially for 3D problems. The modeling of the subsequent wave propagation requires small time steps, which is primarily due to accuracy reasons. Implicit schemes are thus not affordable. Explicit time integration schemes are efficient only for diagonal mass matrices, as in this case no solution of a linear system is required. In this work, a coupled finite element - Non-Uniform Rational B-Spline (FE-NURBS) approach is applied to impact problems. The coupled approach uses an intermediate NURBS layer to compute the contact forces between the contacting bodies discretized by FEs. The advantages of a smooth isogeometric contact formulation are used to compute the contact forces. A segmentation of the contact area is avoided and an efficient element-based integration is used. The impact event is regularized using a mesh dependent nonlinear penalty approach. The penalty function is a polynomial which ensures a smooth transition between the noncontact and the contact state during the impact. For finer meshes, the penalty regularization becomes stiffer while still avoiding artificial oscillations in the contact stresses. Efficient higher order space and time discretizations are used to model the wave propagation. Explicit time integration is combined with higher order spectral element spatial discretization.
Halomonas elongata is a halophilic γ-proteobacterium that synthesizes and accumulates the compatible solute ectoine to cope with osmotic stress in saline environments. Ectoine possesses protecting properties and stabilizes proteins as well as whole cells against stresses like ionizing radiation and cytotoxins. These properties make ectoine a highly demanded ingredient in cosmetics and pharmaceuticals. To date H. elongata is the industrial Producer strain of ectoine, but several metabolic factors for optimum ectoine production remain to be explored.
In this work, we used up to date Metabolic engineering approaches following the ‘Push, Pull, Block – strategy’ to examine targets that contribute to ectoine synthesis. Firstly, the basics of glucose catabolism were inspected to PUSH and enhance carbon flow towards ectoine synthesis. Secondly, lysine biosynthesis was targeted to BLOCK a pathway that is competing for precursors with ectoine synthesis. Thirdly, the mechanosensitive (MS) channels of H. elongata have been examined as possible excretion routes for ectoine. An overexpression of the ectoine excretion channels potentially could PULL out product at the end of ectoine synthesis and increase overall ectoine flux. For the interrogation of central metabolic pathways, we established the new molecular tool CRISPR-mediated interference (CRISPRi) for targeted modulation of gene expression.
PUSH Glucose catabolism through the Entner-Doudoroff (ED) and Emden-Meyerhof-Parnas (EMP) pathway was targeted with CRISPRi and examined on gene expression level for ist response to changing salinity and different carbon sources. Changing salinity did not influence gene expression levels of glucose catabolism but the carbon source glucose triggered glycolysis through the (ED) pathway. When gene expression of the ED pathway was downregulated with CRISPRi, the growth rates remained constant. The observations indicate a metabolic overflow mechanism for glycolysis, in which fluxes are constantly high - even at lower salinity when no resources are demanded for ectoine synthesis. The further analysis of glucose to product conversion rates will advise optimum conditions for future industrial cultivation processes.
BLOCK Lysine biosynthesis was downregulated with CRISPRi, which led to a significant increase in ectoine production. Hence, the blockage of lysine biosynthesis would be a valuable strategy for the optimization of the industrial producer strain in future studies.
PULL MS channels and ectoine regulation are inevitably connected in osmoadaptation. Therefore, ectoine excretion, growth performance and gene expression levels of the MS channels were monitored in steady state conditions and in response to osmotic shock in the wildtype strain and in a MS channel deletion mutant. We observed that the MS channels were essential for the survival of osmotic shock but surprisingly their presence reduced cell growth under high salinity. The MS channels were only partially responsible for ectoine excretion.
Thus, alternative ectoine excretion channels must exist and remain to be explored.
The risk analysis of road tunnels faces a growing complexity in fire scenarios, e.g. caused by new energy carriers. Essentially, such complex scenarios involve many interactions between the tunnel users, the fire source and the safety measures. One example is the alarm of tunnel users either initiated by the perception of smoke or by the fire alarm system. To consider these interactions for the quantification of consequences, e.g. fatalities, risk analysis requires a complex model. However, the complex model can compute in practice only few discrete scenarios due to its high computational cost, whereas risk analysis generally needs the consequences of a high number of random scenarios. Metamodels can solve this contradiction. They are able to approximate the consequences of many random scenarios with low computational cost based on the consequences of few discrete scenarios computed with the complex model. The efficiency of metamodels depends on the required number of these discrete scenarios. In this sense, this dissertation proposes an efficient metamodel within an innovative methodology for risk analysis of road tunnels to allow to consider an increased complexity of scenarios. This metamodel applies the following methods or models: the projection array-based design method specifies the experimental design for the discrete scenarios; the combination of the fire model FDS and the microscopic evacuation model FDS+Evac constitutes the complex model; and moving least squares produces the response surface model. The response surface model approximates the consequences of the random scenarios and therewith introduces an uncertainty, called metamodel uncertainty, which is quantified with the prediction interval method. Additionally, stochastic individual characteristics of tunnel users in discrete scenarios computed with FDS+Evac attribute evacuation uncertainties to the consequences. An original development in this dissertation, the ’direct approach’, directly transfers the evacuation uncertainties of the discrete scenarios to any random scenario. The evaluation of the metamodel in this dissertation shows following results. Firstly, the response surface model sufficiently represents the consequences of the complex model. Secondly, the metamodel uncertainty is also essential for this representation, but the prediction interval method reveals a drawback in the risk analysis. Potential approaches to deal with this drawback are discussed. Finally, the direct approach reproduces the evacuation uncertainty of the complex model which then clearly affects the consequences of random scenarios. Therefore, the consideration of the evacuation uncertainty plays an important role for the risk analysis. Furthermore, the projection array-based design method was adapted in this dissertation with two approaches, namely the combination of the experimental designs for FDS and FDS+Evac as well as their sequential refinement. Both approaches contribute to the efficiency of the metamodel. These results lead to following conclusions. Firstly, the metamodel efficiently integrates the consequences of discrete scenarios into risk analysis and thus allows to consider an increased complexity. Secondly, the metamodel is an advancement for risk analysis not only for road tunnelsbutalsomoregeneralinfiresafetyengineering. Forthesetworeasons,themetamodel might be interesting for other methodologies for risk analysis. In addition, the metamodel is generic and is therefore widely applicable on other issues beside from risk analysis, e.g. to assess the safety of structures related to time-consuming experiments depending on multiple variables.
Die Geräteentwicklungen im Bereich der Niederfeld-NMR-Spektroskopie im vergangenen Jahrzehnt ermöglichen den Einsatz kompakter, portabler Magnete mit geringen Streufeldern in Laborumgebungen und industriellen Produktionsanlagen. Somit werden neue Möglichkeiten für hochauflösende NMR-Experimente zur Reaktionsüberwachung eröffnet. Im Rahmen des EU-Projekts CONSENS wurden die Möglichkeiten dieser Methode umfassend anhand einer technisch bedeutenden Reaktion (elektrophile aromatische Substitutionsreaktionen) evaluiert.
Um die Flexibilität einer kontinuierlichen und modularen Pilotanlage durch Echtzeit- Qualitätskontrolle zu fördern, wurde ein vollständig automatisiertes Online- NMR-Modul entwickelt. Der Einsatz eines kommerziellen Niederfeld-NMR-Geräts im industriellen Umfeld wurde durch die entwickelten Lösungen der automatisierten Datenanlyse sowie durch ein zertifiziertes Sicherheitskonzept für den Betrieb in explosionsgefährdeten Zonen ermöglicht. Neben der Überwachung der Produktqualität wurden Online-NMR-Daten in einem neuen iterativen Optimierungsansatz zur Maximierung des Anlagenertrags eingesetzt und dienten als zuverlässige Referenz für die Kalibrierung eines Nahinfrarot-Spektrometers.
Für die Entwicklung einer robusten Datenauswertung der NMR-Spektren, die dem Anspruch der Flexibilität bei Produktwechseln genügt, wurden zunächst Versuche im Labormaßstab durchgeführt, um eine Datenbasis zu schaffen. In diesen Versuchen wurden die aromatischen Amine Anilin, p-Toluidin und p-Fluoranilin mit o-Fluornitrobenzol gekoppelt. Durch Zugabe einer Organolithium-Verbindung (Li- HMDS) findet ein Protonenaustausch zwischen dem primären Amin und Li-HMDS statt. Dies führt zu einer hohen Reaktionsenthalpie und instabilen Aryllithium-Verbindungen. Die Reaktionen wurden hinsichtlich anfallender Zwischenprodukte mittels Hochfeld-NMR-Spektroskopie analysiert.
Nachfolgend wurden die Reaktionen sowohl im Semi-Batch-Verfahren als auch im kontinuierlichen Laborbetrieb mit Online-Niederfeld-NMR-Spektroskopie und Online- Hochfeld-NMR-Spektroskopie untersucht. Da die gemessenen NMR-Spektren besonders im aromatischen Spektralbereich hohe Signalüberlappungen der Reaktanden aufweisen, wurden chemometrische Modelle entwickelt und anhand der Hochfeld-NMR-Methode validiert. Die verwendeten Durchflusszellen für die Niederfeld-NMR-Spektroskopie wurden hinsichtlich ihrer Anwendbarkeit für quantitative Messungen im kontinuierlichen Durchfluss untersucht. Es konnte gezeigt werden, dass Messungen mit einer additiv gefertigten Keramikdurchflusszelle prinzipiell möglich sind.
The present work is intended to make a contribution to the monitoring of civil engineering structures. The detection of damage to structures is based on the evaluation of spatially and temporally distributed hybrid measurements. The acquired data can be evaluated purely geometrically or physically. It is preferable to do the latter, since the cause of damage can be determined by means of geometrical-physical laws in order to be able to intervene in time and ensure the further use of the structures. For this reason, the continuum mechanical field equations in conjunction with the finite element method and hybrid measurements are combined into a single evaluation method by the adjustment calculation. This results in two challenges.
The first task deals with the relationship between the finite element method and the method of least squares. The finite element method solves certain problem classes, which are described by a system of elliptical partial differential equations. Whereas the method of least squares solves another class of problems, which is formulated as an overdetermined system of equations. The striking similarity between both methods is known since many decades. However, it remains unresolved why this resemblance exists. The contribution is to clarify this by examining the variational calculus, especially with regard to its methodological procedure. Although the well-known Gauss-Markov model within the method of least squares and the finite element method solve inherently different problem classes, it is shown that both methods can be derived by following the same methodological steps of the variational calculus. From a methodical viewpoint, this implies that both methods are not only similar, but actually the same. In addition, it is pointed out where a possible cross-connection to other methods exists.
The second task introduces a Measurement- and Model-based Structural Analysis (MeMoS) by integrating the finite element method into the adjustment calculation. It is shown in numerical examinations how this integrated analysis can be used for parameter identification of simple as well as arbitrarily shaped structural components. Based on this, it is examined with which observation types, with which precision and at which location of the structure these measurements must be carried out in order to determine the material parameters as precisely as possible. This serves to determine an optimal and economic measurement set-up. With this integrated analysis, a substitute model of a geometrically complex structure can also be determined. The issue of the detection and localisation of damage within a structure is studied by means of this structural analysis. The Measurement and Model-based Structural Analysis is validated using two different test setups, an aluminum model bridge and a bending beam.
The present work is intended to make a contribution to the monitoring of civil engineering structures. The detection of damage to structures is based on the evaluation of spatially and temporally distributed hybrid measurements. The acquired data can be evaluated purely geometrically or physically. It is preferable to do the latter, since the cause of damage can be determined by means of geometrical-physical laws in order to be able to intervene in time and ensure the further use of the structures. For this reason, the continuum mechanical field equations in conjunction with the finite element method and hybrid measurements are combined into a single evaluation method by the adjustment calculation. This results in two challenges.
The first task deals with the relationship between the finite element method and the method of least squares. The finite element method solves certain problem classes, which are described by a system of elliptical partial differential equations. Whereas the method of least squares solves another class of problems, which is formulated as an overdetermined system of equations. The striking similarity between both methods is known since many decades. However, it remains unresolved why this resemblance exists. The contribution is to clarify this by examining the variational calculus, especially with regard to its methodological procedure. Although the well-known Gauss-Markov model within the method of least squares and the finite element method solve inherently different problem classes, it is shown that both methods can be derived by following the same methodological steps of the variational calculus. From a methodical viewpoint, this implies that both methods are not only similar, but actually the same. In addition, it is pointed out where a possible cross-connection to other methods exists.
The second task introduces a Measurement- and Model-based Structural Analysis (MeMoS) by integrating the finite element method into the adjustment calculation. It is shown in numerical examinations how this integrated analysis can be used for parameter identification of simple as well as arbitrarily shaped structural components. Based on this, it is examined with which observation types, with which precision and at which location of the structure these measurements must be carried out in order to determine the material parameters as precisely as possible. This serves to determine an optimal and economic measurement set-up. With this integrated analysis, a substitute model of a geometrically complex structure can also be determined. The issue of the detection and localisation of damage within a structure is studied by means of this structural analysis. The Measurement and Model-based Structural Analysis is validated using two different test setups, an aluminum model bridge and a bending beam.