Qucosa – Hemholtz-Zentrum Dresden-Rossendorf
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Annual Report 2009 - Institute of Safety Research
Get PDFThe Institute of Safety Research (ISR) is one of the six Research Institutes of Forschungszentrum Dresden-Rossendorf e.V. (FZD), which is a member institution of the Wissenschaftsgemeinschaft Gottfried Wilhelm Leibniz (Leibnizgemeinschaft). Together with the Institutes of Radiochemistry and Radiation Physics, ISR implements the research programme „Nuclear Safety Research“, which is one of the three scientific programmes of FZD. The programme includes two main topics, i. e. “Safety Research for Radioactive Waste Disposal” and “Safety Research for Nuclear Reactors”
Two-phase flow experiments in a model of the hot leg of a pressurised water reactor
Get PDFIn order to investigate the two-phase flow behaviour in a complex reactor-typical geometry and to supply suitable data for CFD code validation, a model of the hot leg of a pressurised water reactor was built at FZD. The hot leg model is operated in the pressure chamber of the TOPFLOW test facility, which is used to perform high-pressure experiments under pressure equilibrium with the inside atmosphere of the chamber. This technique makes it possible to visualise the two-phase flow through large windows, also at reactor-typical pressure levels. In order to optimise the optical observation possibilities, the test section was designed with a rectangular cross-section.
Experiments were performed with air and water at 1.5 and 3.0 bar at room temperature as well as with steam and water at 15, 30 and 50 bar and the corresponding saturation temperature (i.e. up to 264°C). The total of 194 runs are divided into 4 types of experiments covering stationary co-current flow, counter-current flow, flow without water circulation and transient counter-current flow limitation (CCFL) experiments.
This report provides a detailed documentation of the experiments including information on the experimental setup, experimental procedure, test matrix and on the calibration of the measuring devices. The available data is described and data sheets were arranged for each experiment in order to give an overview of the most important parameters. For the cocurrent flow experiments, water level histograms were arranged and used to characterise the flow in the hot leg. In fact, the form of the probability distribution was found to be sensitive to the boundary conditions and, therefore, is useful for the CFD comparison.
Furthermore, the flooding characteristics of the hot leg model plotted in terms of the classical Wallis parameter or Kutateladze number were found to fail to properly correlate the data of the air/water and steam/water series. Therefore, a modified Wallis parameter is proposed, which takes the effect of viscosity into account
Schlussbericht zum BMBF-Vorhaben \"Entwicklung und Erprobung neuer Instrumente zur Bildung von Verwertung- und Transfernetzen\" NanoFoto - Neue Wege zur verwertungsorientierten Netzwerkbildung in der Nanobiotechnologie
Get PDFBis zu 95 % der Wirkstoffe von Arzneimittel der Humanmedizin werden unverändert ausgeschieden oder gelangen über die täglichen Hygiene in den Wasserkreislauf. Die meisten Substanzen werden sehr schnell und vollständig abgebaut oder liegen in Konzentrationen vor, in denen sie keine Gefährdung für die Umwelt und den Menschen darstellen. Im Gegensatz dazu gibt es aber auch Substanzen, die nur sehr schwer abgebaut werden können (persistent sind) und für die bereits negative Langzeiteffekte in umweltrelevanten Konzentrationen für Tiere nachgewiesen wurden. Ein Beispiel dafür ist der schmerzstillende Wirkstoff Diclofenac. Aus diesem Grund und wegen der guten Kenntnislage hinsichtlich Vorkommen, Abbauprodukte und Analytik wurde Diclofenac als Referenzverbindung für die Experimente im Rahmen dieses Projekts verwendet. Aufgrund der geringen Konzentration von Diclofenac in Wasser und der chemischen Stabilität von Diclofenac sowie einiger anderer Spurenstoffe sind herkömmliche Wasserbehandlungsverfahren, wie sie derzeit in Kläranlangen verwendet werden, ineffizient oder zu teuer. Deshalb gibt es zahlreiche Bemühungen, alternative und umweltschonende Behandlungsverfahren zur Entfernung von Arzneimittelrückständen aus Wasser zu entwickeln, die einen vollständigen Abbau der Rückstände ermöglichen. Idealerweise sollten technische Lösungen zur Verfügung stehen, die gegebenenfalls in jedem Land der Erde einsetzbar wären. Der in diesem Projekt verfolgte Ansatz zur Entwicklung fotokatalytischer Schichten, die idealerweise bereits bei Tageslicht eine ausreichend hohe Aktivität aufweisen, ist besonders interessant, da es nach Optimierung weder des zusätzlichen Einsatzes von Chemikalien noch des Einsatzes von Energie bedarf. So werden durch die Bestrahlung des Katalysators (z.B. ZnO, TiO2) mit künstlichem UV-Licht, perspektifisch aber mit UV-A-Strahlung der Sonne sowohl Wasser als auch Luftsauerstoff zu reaktiven Hydroxylradikalen umgesetzt, die letztendlich die unspezifischen Spaltung organischer Verbindungen im Wasser bewirken. Voraussetzung für die Optimierung hinsichtlich katalytischer Aktivität und Empfindlichkeit gegenüber Tageslicht ist ein Herstellungsverfahren, das die Optimierung der fotokatalytischen Schichten bezüglich verschiedener Parameter (optimale Größe, enge Größenverteilung, Möglichkeit der einfachen Dotierung, Verhinderung der Agglomeration bei gleichzeitiger dauerhafter Immobilisierung) erlaubt. Diesbezüglich besonders aussichtsreich ist die Verwendung von hoch geordneten bakteriellen Hüllproteinen sogenannten „surface-layer“ (S-Layer)-Proteinen, die sowohl eine einfache Herstellung von fotokatalytisch aktiven Nanopartikeln aus verschiedenen Elementen erlauben, als auch zur Beschichtung verschiedener Materialien geeignet sind. Ein Ziel im Projekt ist die Herstellung von reinen und dotierten ZnO und TiO2-Nanopartikeln zur Eliminierung von Diclofenac aus Wasser (siehe Abbildung 1). Dabei dienen S-Layer verschiedener Bakterien und damit Proteinschichten mit unterschiedlichen Symmetrien, Gitterabständen und Porengröße als Template für die Herstellung von Nanopartikeln verschiedener aber definierter Größe.
Darüber hinaus werden die S-Layer im Projekt als Trenn- und Immobilisierungsschicht für die erzeugten Nanopartikel genutzt. Letzteres vor allem zur Verhinderung einer Agglomeration und des Austrags der Nanopartikel, was beides einen Verlust der katalytischen Aktivität entsprechender Schichten bedeuten würde. Als Träger werden im Rahmen des Projekts verschiedene in technischen Anwendungen genutzte Materialien dahin gehend überprüft, in wie weit sich S-Layer darauf abscheiden lassen und stabile Schichten ausbilden und darauf aufbauend ein Trägermaterial für die Herstellung fotokatalytisch aktiver Beschichtungen ausgewählt. Gleichzeitig war es Ziel des Projektes, die Biomassegewinnung hinsichtlich eines Upscalings und
hinsichtlich der Kosten zu optimieren.
Ausgehend von dieser konkreten wissenschaftlichen Fragestellung war es auch Ziel des Projektes, ein verwertungsorientiertes Netzwerk aufzubauen. Dies vor allem zur Sicherung der Fortentwicklung der neuen Materialien und der Weiterführung der begonnenen Arbeiten in dem konkreten Forschungsgebiet mit dem Ziel der Entwicklung eines marktreifen Produktes aber auch zur Etablierung einer dauerhaften Kooperation zwischen den verschiedenen Forschungs- und Industriepartnern. Diese Ziele sollten insbesondere über eine Vernetzung von Instituten innerhalb der Leibniz-Gemeinschaft, weiteren regionalen und überregionalen Forschungseinrichtungen sowie Industriepartnern erreicht werden. Die sehr gute gerätetechnische Ausstattung, die im vorliegenden Fall über die Projektmittel erreicht wurde, war nicht nur Voraussetzung zur Durchführung der geplanten Forschungs- und Entwicklungsarbeiten und zur Herstellung von Materialien im kleintechnischen Maßstab, sondern erhöhte auch die Attraktivität des Teams als Projektpartner weiter und nachhaltig. Erfahrungen aus dem Projekt und dem Prozess der Netzwerkbildung sollen insbesondere unter Einbeziehung der Geschäftsstelle der Leibniz-Gemeinschaft zur Entwicklung eines Prozessleitfadens für die Bildung von Verwertungs- und Transfernetzwerken innerhalb der Leibniz-Gemeinschaft genutzt werden
Bi-Annual Report 2007/08 - Rossendorf Beamline at ESRF (ROBL-CRG)
Get PDFThe Rossendorf Beamline (ROBL) - located at BM20 of the European Synchrotron Radiation Facility (ESRF) in Grenoble, France - is in operation since 1998. This 6th report covers the period from January 2007 to December 2008. In these two years, 50 peerreviewed papers have been published based on experiments done at the beamline. The average citation index, which increased constantly over the years, has now reached 3.5 (RCH) and 3.0 (MRH), indicating that papers are predominately published in journals with high impact factors. Six exemplary highlight reports on the following pages should demonstrate the scientific strength and diversity of the experiments performed on the two end-stations of the beamline, dedicated to Radiochemistry (RCH) and Materials Research (MRH).
Demand for beamtime remains very high as in the previous years, with an average oversubscription rate of 1.8 for ESRF experiments. The attractiveness of our beamline is based upon the high specialization of its two end-stations. RCH is one of only two stations in Europe dedicated to x-ray absorption spectroscopy of actinides and other radionuclides. The INE beamline at ANKA provides superior experimental flexibility and extends to lower energies, including important elements like P and S. In contrast, ROBL-RCH provides a much higher photon flux, hence lower detection limits crucial for environmental samples, and a higher energy range extending to elements like Sb and I. Therefore, both beamlines are highly complementary, covering different aspects of radiochemistry research. Once the MARS beamline at SOLEIL is ready to run radionuclides (>2010), it will cover a third niche (Materials Science of actinides, including irradiated fuel) not accessible for the two other beamlines.
The Materials Research Hutch MRH has realized an increasing number of in-situ investigations in the last years. On the one hand thin film systems were characterized during magnetron sputtering. On the other hand diffraction experiments under controlled atmosphere were performed. A high variety of experimental parameters was covered by varying pressure, temperature and atmospheric compositions including highly reactive gases. Furthermore structural investigations were combined with electrical conductivity measurements. These kind of in-situ experiments are the key to monitor and understand reaction mechanism or the influence of process parameters, which are again the basis to tailor materials properties on demand. The core competences of MRH are these experimental possibilities, which make it unique among other diffraction beamlines. In fall 2007, ROBL was reviewed by an international panel on behalf of the ESRF. The very positive panel report recommended a renewal of the contract between ESRF and FZD for the next five years, and a major upgrade of critical optical components of the beamline to keep ROBL competitive for the next decade. The FZD will provide 2 Mio € from 2009 to 2011 for this upgrade, which will be performed in parallel to the major upgrade of the ESRF to minimize the downtime. According to the current plans of the ESRF, our users have to expect that ROBL will have only limited or no operation for several months from August 2011 on.
Since July 2004 the beamline is a member of the pooled facilities of ACTINET – European Network of Excellence. In the reported period, RCH has provided 27 % of its inhouse beamtime to perform 11 ACTINET experiments. The success of ACTINET within FP-6 has now led to a renewal of ACTINET within FP-7, running until end of 2011
The Mobilization of Actinides by Microbial Ligands Taking into Consideration the Final Storage of Nuclear Waste - Interactions of Selected Actinides U(VI), Cm(III), and Np(V) with Pyoverdins Secreted by Pseudomonas fluorescens and Related Model Compounds (Final Report BMBF Project No.: 02E9985)
Get PDFThe groundwater bacterium Pseudomonas fluorescens (CCUG 32456) isolated at a depth of 70 m in the Äspö Hard Rock Laboratory secretes a pyoverdin-mixture with four main components (two pyoverdins and two ferribactins). The dominant influence of the pyoverdins of this mixture could be demonstrated by an absorption spectroscopy study. The comparison of the stability constants of U(VI), Cm(III), and Np(V) species with ligands simulating the functional groups of the pyoverdins results in the following order of complex strength: pyoverdins (PYO) > trihydroxamate (DFO) > catecholates (NAP, 6HQ) > simple hydroxamates (SHA, BHA). The pyoverdin chromophore functionality shows a large affinity to bind actinides. As a result, pyoverdins are also able to complex and to mobilize elements other than Fe(III) at a considerably high efficiency. It is known that EDTA may form the strongest actinide complexes among the various organic components in nuclear wastes. The stability constants of 1:1 species formed between Cm(III) and U(VI) and pyoverdins are by a factor of 1.05 and 1.3, respectively, larger compared to the corresponding EDTA stability constants. The Np(V)-PYO stability constant is even by a factor of 1.83 greater than the EDTA stability constant. The identified Np(V)-PYO species belong to the strongest Np(V) species with organic material reported so far. All identified species influence the actinide speciation within the biologically relevant pH range. The metal binding properties of microbes are mainly determined by functional groups of their cell wall (LPS: Gram-negative bacteria and PG: Gram-positive bacteria). On the basis of the determined stability constants raw estimates are possible, if actinides prefer to interact with the microbial cell wall components or with the secreted pyoverdin bioligands. By taking pH 5 as an example, U(VI)-PYO interactions are slightly stronger than those observed with LPS and PG. For Cm(III) we found a much stronger affinity to aqueous pyoverdin species than to functional groups of the cell wall compartments. A similar behavior was observed for Np(V). This shows the importance of indirect interaction processes between actinides and bioligands secreted by resident microbes
Evolution of Ion-Induced Ripple Patterns - Anisotropy, nonlinearity, and scaling
Get PDFThis thesis addresses the evolution of nanoscale ripple patterns on solid surfaces during low-energy ion sputtering. Particular attention is paid to the long-time regime in which the surface evolution is dominated by nonlinear processes. This is explored in simulation and experiment.
In numerical simulations, the influence of anisotropy on the evolution of the surface patterns in the anisotropic stochastic Kuramoto-Sivashinsky (KS) equation with and without damping is studied. For a strong nonlinear anisotropy, a 90 rotation of the initial ripple pattern is observed and explained by anisotropic renormalization properties of the anisotropic KS equation. This explanation is supported by comparison with analytical predictions. In contrast to the isotropic stochastic KS equation, interrupted ripple coarsening is found in the presence of low damping. This coarsening seems to be a nonlinear anisotropy effect that occurs only in a narrow range of the nonlinear anisotropy parameter.
Ex-situ atomic force microscopy (AFM) investigations of Si(100) surfaces sputtered with sub-keV Ar ions under oblique ion incidence show the formation of a periodic ripple pattern. This pattern is oriented normal to the direction of the ion beam and has a periodicity well below 100 nm. With increasing ion fluence, the ripple pattern is superposed by larger corrugations that form another quasi-periodic pattern at high fluences.
This ripple-like pattern is oriented parallel to the direction of the ion beam and has a periodicity of around one micrometer. Interrupted wavelength coarsening is observed for both patterns. A dynamic scaling analysis of the AFM images shows the appearance of anisotropic scaling at large lateral scales and high fluences. Based on comparison with the predictions of different nonlinear continuum models, the recent hydrodynamic model of ion erosion, a generalization of the anisotropic KS equation, is considered as a potentially powerful continuum description of this experiment.
In further in-situ experiments, the dependence of the dynamic scaling behavior of the sputtered Si surface on small variations of the angle of incidence is investigated by grazing incidence small angle X-ray scattering (GISAXS). A transition from strongly anisotropic to isotropic scaling is observed. This indicates the presence of at least two fixed points in the system, an anisotropic and an isotropic one. The dynamic scaling exponents of the isotropic fixed point are in reasonable agreement with those of the Kardar-Parisi-Zhang (KPZ) equation. It remains to be seen whether the hydrodynamic model is able to show such a transition from anisotropic to isotropic KPZ-like scaling
An Investigation of Target Poisoning during Reactive Magnetron Sputtering
Get PDFObjective of the present work is a broad investigation of the so called target poisoning during magnetron deposition of TiN in an Ar/N2 atmosphere. Investigations include realtime in-situ ion beam analysis of nitrogen incorporation at the Ti sputter target during the deposition process and the analysis of particle uxes towards and from the target by means of energy resolved mass spectrometry. For experiments a planar, circular DC magnetron, equipped with a 2 inch titanium target was installed in an ultrahigh vacuum chamber which was attached to the beam line system of a 5 MV tandem accelerator. A manipulator allows to move the magnetron vertically and thereby the lateral investigation of the target surface. During magnetron operation the inert and reactive gas flow were adjusted using mass flow controllers resulting in an operating pressure of about 0.3 Pa. The argon flow was fixed, whereas the nitrogen flow was varied to realize different states of target poisoning. In a fi?rst step the mass spectrometer was used to verify and measure basic plasma properties e.g. the residual gas composition, the behavior of reactive gas partial pressure, the plasma potential and the dissociation degree of reactive gas molecules. Based on the non-uniform appearance of the magnetron discharge further measurements were performed in order to discuss the role of varying particle fluxes across the target during the poisoning process. Energy and yield of sputtered particles were analyzed laterally resolved, which allows to describe the surface composition of the target. The energy resolving mass spectrometer was placed at substrate position and the target surface was scanned by changing the magnetron position correspondingly. It was found, that the obtained energy distributions (EDF) of sputtered particles are influenced by their origin, showing signi?ficant differences between the center and the erosion zone of the target. These results are interpreted in terms of laterally different states of target poisoning, which results in a variation of the surface binding energy. Consequently the observed energy shift of the EDF indicates the metallic or already poisoned fraction on target surface. Furthermore the EDF's obtained in reactive sputtering mode are broadened. Thus a superposition of two components, which correspond to the metallic and compound fractions of the surface, is assumed. The conclusion of this treatment is an discrete variation of surface binding energy during the transition from metallic to compound target composition. The reactive gas target coverage as derived from the sputtered energy distributions is in reasonable agreement with predictions from model calculations. The target uptake of nitrogen was determined by means of ion beam analysis using the 14N(d, )12C nuclear reaction. Measurements at varying nitrogen gas flow directly demonstrate the poisoning eff?ect. The reactive gas uptake saturates at a maximum nitrogen areal density of about 1.1016 cm-2 which corresponds to the stoichiometric limit of a 3 nm TiN layer. At sufficiently low reactive gas flow a scan across the target surface discloses a pronounced lateral variation of target poisoning, with a lower areal density in the target race track compared to the target center and edge. Again the findings are reproduced by model calculations, which confirm that the balance of reactive gas injection and sputter erosion is shifted towards erosion in the race track. Accomplished computer simulations of the reactive sputtering process are similar to Berg's well known model. Though based on experimental findings the algorithm was extended to an analytical two layer model which includes the adsorption of reactive gas as well as its different kinds of implantation. A distribution of ion current density across the target diameter is introduced, which allows a more detailed characterization of the processes at the surface. Experimental results and computer simulation have shown that at sufficiently low reactive gas flow, metallic and compound fractions may exist together on the target surface, which is in contradiction to previous simulations, where a homogeneous reactive gas coverage is assumed. Based on the results the dominant mechanisms of nitrogen incorporation at different target locations and at varying reactive gas admixture were identified
Fast Digitizing and Digital Signal Processing of Detector Signals
Get PDFA fast-digitizer data acquisition system recently installed at the neutron time-of-flight experiment nELBE, which is located at the superconducting electron accelerator ELBE of Forschungszentrum Dresden-Rossendorf, is tested with two different detector types. Preamplifier signals from a high-purity germanium detector are digitized, stored and finally processed. For a precise determination of the energy of the detected radiation, the moving-window deconvolution algorithm is used to compensate the ballistic deficit and different shaping algorithms are applied. The energy resolution is determined in an experiment with γ-rays from a 22Na source and is compared to the energy resolution achieved with analogously processed signals. On the other hand, signals from the photomultipliers of barium fluoride and plastic scintillation detectors are digitized. These signals have risetimes of a few nanoseconds only. The moment of interaction of the radiation with the detector is determined by methods of digital signal processing. Therefore, different timing algorithms are implemented and tested with data from an experiment at nELBE. The time resolutions achieved with these algorithms are compared to each other as well as to reference values coming from analog signal processing. In addition to these experiments, some properties of the digitizing hardware are measured and a program for the analysis of stored, digitized data is developed. The analysis of the signals shows that the energy resolution achieved with the 10-bit digitizer system used here is not competitive to a 14-bit peak-sensing ADC, although the ballistic deficit can be fully corrected. However, digital methods give better result in sub-ns timing than analog signal processing