Wissenschaftliche Artikel der BAM
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- 1 Analytische Chemie; Referenzmaterialien (51)
- 8 Zerstörungsfreie Prüfung (51)
- 6 Materialchemie (37)
- 7 Bauwerkssicherheit (35)
- 4 Material und Umwelt (18)
- 5 Werkstofftechnik (16)
- 6.3 Strukturanalytik (13)
- 8.5 Röntgenbildgebung (12)
- 9 Komponentensicherheit (12)
- 1.2 Biophotonik (11)
We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low.
Dual-phase membranes for high-temperature carbon dioxide Separation have emerged as promising technology to mitigate anthropogenic greenhouse gases emissions, especially as a pre- and post-combustion separation technique in coal burning power plants. To implement These membranes industrially, the carbon dioxide permeability must be improved. In this study, Ce_(0.8) Sm_(0.2) O_(2-d) (SDC) and Ce_(0.8)Sm_(0.19)Fe_(0.01)O_(2-d) (FSDC) ceramic powders were used to form the skeleton in dual-Phase membranes. The use of MgO as an environmentally friendly pore generator allows control over the membrane porosity and microstructure in order to compare the effect of the membrane’s ceramic phase. The ceramic powders and the resulting membranes were characterized using ICP-OES, HSM, gravimetric analysis, SEM/EDX, and XRD, and the carbon dioxide flux density was quantified using a high-temperature membrane permeation setup. The carbon dioxide permeability slightly increases with the addition of iron in the FSDC membranes compared to the SDC membranes mainly due to the reported scavenging effect of iron with the siliceous impurities, with an additional potential contribution of an increased crystallite size due to viscous flow sintering. The increased permeability of the FSDC system and the proper microstructure control by MgO can be further extended to optimize carbon dioxide permeability in this membrane system.
Gasoline adulteration is a frequent problem world-wide, because of the chance of quick, maximized profits. However, addition of cheaper ethanol or hydrocarbons like kerosene does not only result in economic damage but also poses problems for vehicles and the environment. To enable law enforcement forces, customers or enterprises to uncover such a fraudulent activity directly upon suspicion and without the need to organize for sampling and laboratory analysis, we developed a simple strip-based chemical test. Key to the favorable performance was the dedicated materials tailoring, which led to test strips that consisted of a cellulose support coated with silica, passivated with hexamethyldisilazane and functionalized covalently with a molecular probe. The probe fluoresces brightly across a broad solvent polarity range, enabling reliable quantitative measurements and data analysis with a conventional smartphone. The assays showed high reproducibility and accuracy, allowing not only for the detection of gasoline adulteration but also for the on-site monitoring of the quality of commercial E10 gasoline.
We investigate the nearfield dipole mobility of protein membranes in a wide frequency range from 3 kHz to 10 GHz. The results of our nanoscale dielectric images and spectra of bacteriorhodopsin (bR) reveal Debye relaxations with time constants of τ ∼ 2 ns and τ ∼ 100 ns being characteristic of the Dipole moments of the bR retinal and α-helices, respectively. However, the dipole mobility and therefore the protein biophysical function depend critically on the amount of surface water surrounding the protein, and the characteristic mobility in the secondary structure is only observed for humidity levels <30%. Our results have been achieved by adding the frequency as a second fundamental dimension to quantitative dielectric microscopy. The key elements for the success of this advanced technique are the employed heterodyne detection scheme, the broadband electrical signal source, a high frequency optimized cabling, development of calibration procedures and precise finite element modelling. Our study demonstrates the exciting possibilities of broadband dielectric microscopy for the investigation of dynamic processes in cell bioelectricity at the individual molecular level. Furthermore, the technique may shed light on local dynamic processes in related materials science applications like semiconductor Research or nano-electronics.
X-ray reflectivity (XRR) is a powerful and popular scattering technique that can give valuable insight into the growth behavior of thin films. This study Shows how a simple artificial neural network model can be used to determine the thickness, roughness and density of thin films of different organic semiconductors [diindenoperylene, copper(II) phthalocyanine and alpha-sexithiophene] on silica from their XRR data with millisecond computation time and with minimal user input or a priori knowledge. For a large experimental data set of 372 XRR curves, it is shown that a simple fully connected model can provide good results with a mean absolute percentage error of 8–18% when compared with the results obtained by a genetic least mean squares fit using the classical Parratt formalism. Furthermore, current drawbacks and prospects for improvement are discussed.
When handling flammable or toxic liquids or liquefied gases, the occurrence of a leakage and formation of a liquid pool is a scenario to be considered for risk assessment. Several models are available for the estimation of the evaporating mass flow, but only a very reduced number of experimental data is available for Validation purposes.
In the last years, the Federal Institute for Materials Research and Testing (BAM) in Berlin, Germany, carried out pool Evaporation experiments with different substances in basins with a Diameter ranging from 0,50 m to 1 m mainly on open air test sites with a built up (inner city) and a non-built-up (flat terrain) topography, but also in an enclosed space. The resulting experimental data sets cover a range of vapor pressures from 0,1 bar to 0,94 bar.
The aim of this work is to make the füll data set publicly available and to provide a description of the experimental boundary conditions.
Based on these data, a Validation of existing pool Evaporation models has been carried out and eventually led to a new formulation of an evaporation model, which is also presented here, covering the whole ränge from low wind speeds up to high vapor pressures.
The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling.
The movement of the macroscopic magnetic moment in ferromagnetic systems can be described by the Landau-Lifshitz (LL) or Landau-Lifshitz-Gilbert (LLG) equation. These equations are strictly valid only at absolute zero temperature. To include temperature effects a stochastic version of the LL or LLG equation for a spin density of one per unit cell can be used instead. To apply the stochastic LL to micromagnetic simulations, where the spin density per unit cell is generally higher, a conversion regarding simulation cell size and temperature has to be established. Based on energetic considerations, a conversion for ferromagnetic bulk and thin film systems is proposed. The conversion is tested in micromagnetic simulations which are performed with the Object Oriented Micromagnetic Framework (OOMMF). The Curie temperatures of bulk Nickel, Cobalt and Iron systems as well as Nickel thin-film systems with thicknesses between 6.3 mono layer (ML) and 31ML are determined from micromagnetic simulations. The results show a good agreement with experimentally determined Curie temperatures of bulk and thin film systems when temperature scaling is performed according to the presented model.
High resolution analysis of corrosion processes on stainless steels is a challenging task. The application of local electrochemical techniques such as scanning electrochemical microscopy (SECM) has opened new possibilities for the detection of corrosion products and activity on metallic surfaces. However, due to its stochastic nature, the analysis of pitting corrosion requires being at the right place at the right time. Scanning over large areas at a high resolution not only leads to long scan durations but also leaves many short-lived processes undetected. In this paper we present the combined automated operation of SECM and wire multi-electrodes connected to a multi-electrode analyzer (MMA). The inter-electrode currents between 25 wire electrodes connected via zero resistance ammeters (ZRA) are measured by the MMA at open circuit potential (OCP) and the electrodes reporting anodic currents are detected automatically to be analyzed by means of SECM. The results demonstrate the successful application of this methodology for the detection of unstable and stable pitting processes on 304 stainless steel in a corrosive aqueous environment.
Larvae and adults of Korynetes caeruleus (de Geer 1775) (Coleoptera: Cleridae) were collected from old churches and reared in the laboratory on Anobium punctatum (de Geer 1774) (Coleoptera: Ptinidae). Breeding success of K. caeruleus was low, but basic parameters of this species’ developmental cycle were identifi ed. At 21°C and 75% relative humidity and a fourmonth cold period at 4°C, the development of K. caeruleus from egg to adult appearance lasted 2 years. The pupal stage may be reached and completed after one and a half years. Feeding on larvae of A. punctatum by larvae of K. caeruleus was observed and consisted of a combination of sucking haemolymph and consuming body parts. The sickle-like mandibles of larvae of K. caeruleus penetrate the cuticle of prey larvae; this is followed by pumping and sucking body movements. Adult beetles of A. punctatum were not attacked by K. caeruleus larvae. Feeding behaviour of adult K. caeruleus was not investigated.
Background signals from in situ-formed amorphous carbon, despite not being fully understood, are known to be a common issue in few-molecule surface-enhanced Raman scattering (SERS). Here, discrete gold and silver nanoparticle aggregates assembled by DNA origami were used to study the conditions for the formation of amorphous carbon during SERS measurements. Gold and silver dimers were exposed to laser light of varied power densities and wavelengths. Amorphous carbon prevalently formed on silver aggregates and at high power densities. Time-resolved measurements enabled us to follow the formation of amorphous carbon. Silver nanolenses consisting of three differently-sized silver nanoparticles were used to follow the generation of amorphous carbon at the single-nanostructure level. This allowed observation of the many sharp peaks that constitute the broad amorphous carbon signal found in ensemble measurements. In conclusion, we highlight strategies to prevent amorphous carbon formation, especially for DNA-assembled SERS substrates.
Zuverlässigkeitsbetrachtungen bei der Ultraschallprüfung von Radsatzwellen im Ausbildungsbetrieb
(2019)
Im Rahmen der UT1-M1 Ausbildung im Ausbildungszentrum Wittenberge der DGZfP wurden statistische Untersuchungen am Beispiel der Radsatzwellenprüfung mit Testradsatzwellen durchgeführt. Diese Untersuchungen hatten zum Ziel, die wesentlichen Einflussparameter bei der Prüfung auf das Prüfergebnis zu evaluieren. Dabei wurde unter anderem die intrinsische Fähigkeit des Prüfverfahrens zum Auffinden verschiedener Reflektorgeometrien ermittelt. Die Ergebnisse der Handprüfung wurden mit Ergebnissen mechanisierter Prüfungen verglichen. Im Rahmen der Zuverlässigkeitsbetrachtung wurden die Probability of Detection (POD) und die Nachweisgrenzen ermittelt.
Ziel dieser Arbeit war es auch, menschliche und organisatorische Einflussfaktoren auf die Ultraschall-Handprüfung von Radsatzwellen zu identifizieren, um Empfehlungen zur Optimierung der Ausbildung auszuarbeiten. Dazu wurden prüfungsbezogene Risiken in der Praxis mittels Fehlzustandsart- und –auswirkungsanalyse (FMEA) analysiert sowie von den Prüfern empfundene Probleme während der Ausbildung und in der Praxis mittels Fragebogen identifiziert. Die Ergebnisse der FMEA haben gezeigt, dass während des gesamten Prozesses Fehler auftreten können, für die Gegenmaßnahmen getroffen und implementiert werden sollten. Aus den Hinweisen und Erkenntnissen wurden einige Empfehlungen zur Optimierung der Ausbildung erarbeitet.
Bei der mechanisierten Prüfung von verlegten Eisenbahnschienen mit Schienenprüfzügen werden große Prüfdatenmengen mit einer komplexen Prüfkopfanordnung in kurzer Zeit bei hohen Prüfgeschwindigkeiten aufgenommen. Der Typ und der Zustand des Gleises kann während der Prüfung in schnellem Wechsel streckenabhängig variieren, z.B. unterschiedliche Schienentypen oder Abnutzung sowie beim Durchfahren von Weichenstraßen. Der logistische Aufwand diese Prüfung insgesamt durchzuführen ist dabei sehr hoch und eine Wiederholung der Prüfung in einem kurzen Zeitintervall nicht möglich.
Es werden während der Prüfdatenaufnahme bereits Datenreduktionsverfahren, Rekonstruktionsverfahren und Online-Parametervariationen eingesetzt, um die Ergebnisdaten zum einen in Ihrer Menge zu begrenzen zum anderen auf die lokalen Geometrie- und Zustandsänderungen des Prüfobjektes Schiene zu reagieren.
Im Regelwerk EN 16729-1 „Zerstörungsfreie Prüfung an Schienen im Gleis -Teil 1: Anforderungen an Ultraschallprüfungen und Bewertungsgrundlagen“ werden Bezugsreflektoren definiert, um die Leistung automatisierter Ultraschallsysteme für die Schienenprüfung zu verifizieren.
Um die Einflüsse der komplexen Randbedingungen der mechanisierten Schienenprüfung auf das Prüfergebnis evaluieren zu können, wurde ein Softwarewerkzeug erarbeitet, mit dem eine Prüffahrt auf einer Schiene simuliert werden kann. Basierend auf der Datenaufnahme mit dem Glassy-Rail-Diagramm können alle relevanten Prüfparameter und Artefakte in Schienen sowie Störeinflüsse bei der Simulation berücksichtigt werden.
Large-pore ordered mesoporous silica (OMS) COK-12, analogous to the well-known SBA-15, but synthesized in a more environmentally friendly way and exhibiting a shorter plate-like structure, was grafted with different amounts of graphene oxide (GO) for the first time in an inexpensive and rapid process, that was successfully upscaled. Samples were examined with nitrogen sorption analysis, SAXS, Raman spectroscopy, XPS, and zeta potential analysis. Adsorption experiments with the cationic dye methylene blue (MB) were conducted on the grafted materials and on pure COK-12, taking into account the influence of initial dye concentration (30–600 mg L-1), adsorbent dosage (0.2–14 g L-1), contact time (0.3–300 min), solution pH (4 10), and influence of salts and temperature (0–1 M NaCl, 80 C) to simulate industrial dye effluent. The adsorption process was found to be represented best by the Langmuir isotherm model, i.e., adsorption is a monolayer process. The calculated maximum Adsorption capacities were found to be 20.2 and 197.5 mg g-1 at dosages of 5 and 0.5 g L-1 for pure COK-12 and COK-12 grafted with 50 wt% GO, respectively, at pH 5.65 and MB concentration of 100 mg L-1.
Adsorption kinetics were found to follow the pseudo-second order model, i.e., chemisorption is the rate controlling step. The adsorption performances could be well preserved at simulated dye effluent.
Desorption was found to be most effective with hydrochloric acid. The COK-12 grafted with GO presented in this work shows superior adsorption properties in comparison to other grafted OMS materials. In addition, grafting with GO remarkably improved the stability of COK-12 in aqueous solution.
The identification of the dynamic behavior of structures, like bridges and towers, is relevant to address multiple issues. In many cases the dynamic parameters should be acquired only once or at a frequency that doesn’t justify the installation of distinct vibration sensors for a long-term monitoring. To identify modal frequencies of a structure, a drone based mobile sensing platform has been implemented. This sensing platform measures the relative displacement be-tween the structure and the drone, which also shows a strong dynamic behavior under wind tur-bulences. By regarding the dynamic model of the drone and additional measurements at the dis-tance sensor the absolute movement of the structure can be estimated based on the measured relative distance. This time domain data is a suitable input for various operational modal analysis algorithms. The system has been used to identify the dynamic properties of test and real structure, like a 1.5 MW wind turbine tower.
We present results demonstrating several beneficial effects on distributed fiber optic vibration sensing (DVS) functionality and performance resulting from utilizing standard single mode optical fiber (SMF) with femtosecond laser-inscribed equally-spaced simple scattering dots. This modification is particularly useful when using traditional single-wavelength amplitude-based coherent optical time domain reflectometry (C-OTDR) as sensing method. Local sensitivity is increased in quasi-distributed interferometric sensing zones which are formed by the fiber segments between subsequent pairs of the scattering dots. The otherwise nonlinear transfer function is overwritten with that of an ordinary two-beam interferometer. This linearizes the phase response to monotonous temperature variations. Furthermore, sensitivity fading is mitigated and the demodulation of low-frequency signals is enabled. The modification also allows for the quantitative determination of local temperature gradients directly from the C-OTDR intensity traces. The dots’ reflectivities and thus the induced attenuation can be tuned via the inscription process parameters. Our approach is a simple, robust and cost-effective way to gain these sensing improvements without the need for more sophisticated interrogator technology or more complex fiber structuring, e.g., based on ultra-weak FBG arrays. Our claims are substantiated by experimental evidence.
Mesoporous phosphates are a group of nanostructured materials with promising applications, particularly in biomedicine and catalysis. However, their controlled synthesis via conventional template-based routes presents a number of challenges and limitations. Here, we show how to synthesize a mesoporous Magnesium phosphate with a high surface area and a well-defined pore structure through thermal decomposition of a crystalline struvite (MgNH4PO4·6H2O) precursor. In a first step, struvite crystals with various morphologies and sizes, ranging from a few micrometers to several millimeters, had been synthesized from supersaturated aqueous solutions (saturation index (SI) between 0.5 and 4) at ambient pressure and temperature conditions. Afterwards, the crystals were thermally treated at 70–250 °C leading to the release of structurally bound water (H2O) and ammonia (NH3). By combining thermogravimetric analyses (TGA), scanning and transmission electron microscopy (SEM, TEM), N2 sorption analyses and small- and wide-angle X-ray scattering (SAXS/WAXS) we show that this decomposition process results in a pseudomorphic transformation of the original struvite into an amorphous Mg-phosphate. Of particular importance is the fact that the final material is characterized by a very uniform mesoporous structure with 2–5 nm wide pore channels, a large specific surface area of up to 300 m2 g−1 and a total pore volume of up to 0.28 cm3 g−1. Our struvite decomposition method is well controllable and reproducible and can be easily extended to the synthesis of other mesoporous phosphates. In addition, the so produced mesoporous material is a prime candidate for use in biomedical applications considering that Magnesium phosphate is a widely used, non-toxic substance that has already shown excellent biocompatibility and biodegradability.
Menschen, die in der gemäßigten Klimazone leben, verbringen bis zu 90% ihres Lebens in Innenräumen. Deshalb hat das Innenraumklima eine sehr große Bedeutung für deren Wohlergehen, Gesundheit und Leistungsfähigkeit. In Deutschland wird ca. 40% der eingesetzten Primärenergie für das Heizen, Kühlen und Klimatisieren der Innenräume verwendet.
Das Forschungsvorhaben hat eine Laufzeit vom Oktober 2013 bis März 2017. Es wird in Kooperation mit der Bundesanstalt für Materialforschung und –prüfung (BAM) und der Hochschule für Technik und Wirtschaft Berlin (HTW Berlin) durchgeführt. Die HTW Berlin koordiniert das Projekt. Die Rheinisch-Westfälische Technische Hochschule Aachen (RWTH) wird teilweise über einen Auftrag in das Projekt integriert.
Ziel des Projektes ist es Baustoffe auf ihre Geruchsemissionen zu untersuchen, um Bauprodukte mit niedrigen Emissionen und Gerüchen identifizieren zu können. Den Verbraucherinnen und Verbrauchern wird somit die Möglichkeit gegeben emissions- und geruchsarme Baustoffe zu wählen.
Die Aufgabenstellung des Projektes ist nachfolgend aufgeführt:
Arbeitspaket 1: Geruchsmessung bei Produkten mit dem Blauen Engel (siehe Kapitel 4 und 5);
Arbeitspaket 2: Untersuchung von Vergleichsmaßstäben (siehe Kapitel 6);
Arbeitspaket 3: Untersuchung der Linearität der Acetonskala (siehe Kapitel 7);
Arbeitspaket 4: Erstellung einer Produktdatenbank (siehe Kapitel 8).
Die Geruchsuntersuchung ist in den Vergabekriterien für den „Blauen Engel“ für textile Bodenbeläge (RAL UZ-128) eingebunden worden. Aus den weiteren Untersuchungen sind für die Normung wichtige Erkenntnisse erarbeitet worden.
Structural modularity of polymer frameworks is a key advantage of covalent organic polymers, however, only C, N, O, Si and S have found their way into their building blocks so far. Here, we expand the toolbox available to polymer and materials chemists by one additional nonmetal, phosphorus. Starting with a building block that contains a λ⁵‐phosphinine (C₅P) moiety, we evaluate a number of polymerisation protocols, finally obtaining a π‐conjugated, covalent phosphinine‐based framework (CPF‐1) via Suzuki‐Miyaura coupling. CPF‐1 is a weakly porous polymer glass (72.4 m2 g‐1 N2 BET at 77 K) with green fluorescence (λmax 546 nm) and extremely high thermal stability. The polymer catalyzes hydrogen evolution from water under UV and visible light irradiation without the need for additional co‐catalyst at a rate of 33.3 μmol h‐¹ g‐¹. Our results demonstrate for the first time the incorporation of the phosphinine motif into a complex polymer framework. Phosphinine‐based frameworks show promising electronic and optical properties that might spark future interest in their applications in light‐emitting devices and heterogeneous catalysis.