Wissenschaftliche Artikel der BAM
Filtern
Erscheinungsjahr
Dokumenttyp
Sprache
- Englisch (2295) (entfernen)
Schlagworte
- Additive manufacturing (69)
- Fluorescence (56)
- Nanoparticles (48)
- SAXS (46)
- Concrete (45)
- Corrosion (37)
- MALDI-TOF MS (37)
- Ultrasound (37)
- Quantum yield (36)
- Non-destructive testing (33)
Organisationseinheit der BAM
- 6 Materialchemie (442)
- 8 Zerstörungsfreie Prüfung (377)
- 1 Analytische Chemie; Referenzmaterialien (348)
- 7 Bauwerkssicherheit (219)
- 5 Werkstofftechnik (215)
- 9 Komponentensicherheit (213)
- 4 Material und Umwelt (188)
- 6.3 Strukturanalytik (168)
- 8.5 Röntgenbildgebung (127)
- 6.1 Oberflächen- und Dünnschichtanalyse (100)
Paper des Monats
- ja (71)
Solvent annealing is a versatile tool to adjust the shape and morphology of block copolymer (BCP) particles. During this process, polar solvents are often used for block-selective swelling. However, such water-miscible solvents can induce (partial) solubilization of one block in the surrounding aqueous medium, thus, causing complex structural variations and even particle disassembly. To reduce the complexity in morphology control, we focused on toluene as a nonpolar polystyrene-selective solvent for the annealing of striped polystyrene-b-poly(2-vinylpyridine) (PS-b-P2VP) ellipsoids. The selective stretching of PS chains produces unique asymmetric lamellae structures, which translate to an increase in the particle aspect ratio after toluene evaporation. Complete reversibility is achieved by changing to chloroform as a nonselective solvent. Moreover, surfactants can be used to tune block-selective wetting of the particle surface during the annealing; for example, a PS shell can protect the internal lamellae structure from disassembly. Overall, this versatile postassembly process enables the tailoring of the structural features of striped colloidal ellipsoids by only using commercial BCPs and solvents.
Solution doping of commercial polymethyl methacrylate (PMMA) polymer optical fibers (POFs) is presented as a novel approach for preparation of custom cladding-doped POFs (CD-POFs). The presented method is based on a solution-mediated diffusion of dopant molecules into the fiber cladding upon soaking of POFs in a methanol-dopant solution. The method was tested on three different commercial POFs using Rhodamine B as a fluorescent dopant. The dynamics of the diffusion process was studied in order to optimize the doping procedure in terms of selection of the most suitable POF, doping time and conditions. Using the optimized procedure, longer segment of fluorescent CD-POF was prepared and its performance was characterized. Fiber’s potential for sensing and illumination applications was demonstrated and discussed. The proposed method represents a simple and cheap way for fabrication of custom, short to medium length CD-POFs with various dopants.
Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (<5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios.
Solidification Cracking Assessment of LTT Filler Materials by Means of Varestraint Testing and μCT
(2020)
Investigations of the weldability of metals often deal with hot cracking, as one of the most dreaded imperfections during weld fabrication. The hot cracking investigations presented in this paper were carried out as part of a study on the development of low transformation temperature (LTT) weld filler materials. These alloys allow to mitigate tensile residual stresses that usually arise during welding using conventional weld filler materials. By this means, higher fatigue strength and higher lifetimes of the weld can be achieved. However, LTT weld filler materials are for example, high-alloyed Cr/Ni steels that are susceptible to the formation of hot cracks. To assess hot cracking, we applied the standardized modified varestraint transvarestraint hot cracking test (MVT), which is well appropriate to evaluate different base or filler materials with regard to their hot cracking susceptibility. In order to consider the complete material volume for the assessment of hot cracking, we additionally applied microfocus X-ray computer tomography (μCT). It is shown that by a suitable selection of welding and MVT parameter the analysis of the complete 3D hot crack network can provide additional information with regard to the hot cracking model following Prokhorov. It is now possible to determine easy accessible substitute values (e.g., maximum crack depth) for the extent of the Brittleness Temperature Range (BTR) and the minimum critical strain Pmin.
N-Benzyl aroyl-S,N-ketene acetals can be readily synthesized by condensation of aroyl chlorides and N-Benzyl 2-methyl benzothiazolium salts in good to excellent yields, yielding a library of 35 chromophores with bright solid-state emission and aggregation-induced emission characteristics.
Varying the substituent from electron-donating to electronwithdrawing enables the tuning of the solid-state emission Color from deep blue to red.
Thermal decomposition of [Co(NH₃)₆][Fe(C₂O₄)₃]∙3H₂O in argon atmosphere, at a low heating rate (3°/min), and in large amounts of the initial complex (~0.1 mole), has been studied. It was possible to distinguish four decomposition steps upon heating: In the temperature range of 50⁻100 °C-the loss of crystal water; 100⁻190 °C-stability region of dehydrated complex; 230⁻270 °C-the range of stability of intermediate phase with the formula CoFe(NH₃)₂(C₂O₄)₂; 270⁻350 °C-thermal decomposition of the intermediate with the formation of metallic products and further air oxidation with the formation of Co1.5Fe1.5O₄. Catalytic properties of thermolysis products were tested in the decomposition reaction of H₂O₂ (inactive), oxidation of acetone (average activity), and decomposition of ammonium perchlorate (highly active).
In this study, the wavefield radiated from a building to its surroundings is identified and extracted from M4.6 earthquake recordings collected by sensors installed in a building and on the nearby athletic field in Matera (Italy) using a new approach for soil-structure interaction assessment. The proposed approach for earthquake data analysis combines in an innovative way two methods already used in seismology and engineering seismology: deconvolution and polarization analysis. The approach enables the identification, reconstruction, and characterization of the wavefield radiated from a vibrating building into its surroundings, and the estimation of the amount of energy associated with it. The approach consists of four steps: estimation of the resonant frequencies of the building, deconvolution of the earthquake recordings from a building and its surroundings, identification of the seismic phases, reconstruction of the signal transmitted from the building to its surroundings, and estimation of its energy, and polarization analysis. Analysis of recordings of the M4.6 event highlighted that the motion related to the wavefield radiated from the building to the ground was mostly linearly polarized in the radial and transverse planes, while a clear ellipticity was observed only in the horizontal plane. The wavefield radiated from the building might be dominated by unconventionally polarized surface waves, i.e., quasi-Rayleigh waves or a combination of quasi-Rayleigh and quasi-Love waves. The results indicated that the energy transmitted from the analyzed vibrating building to its surroundings was significant and decreased the ground motion shaking due to the out-of-phase motion.
So near and yet so far: harmonic radar reveals reduced homing ability of Nosema infected honeybees
(2014)
Pathogens may gain a fitness advantage through manipulation of the behaviour of their hosts. Likewise, host behavioural changes can be a defence mechanism, counteracting the impact of pathogens on host fitness. We apply harmonic radar technology to characterize the impact of an emerging pathogen - Nosema ceranae (Microsporidia) - on honeybee (Apis mellifera) flight and orientation performance in the field. Honeybees are the most important commercial pollinators. Emerging diseases have been proposed to play a prominent role in colony decline, partly through sub-lethal behavioural manipulation of their hosts. We found that homing success was significantly reduced in diseased (65.8%) versus healthy foragers (92.5%). Although lost bees had significantly reduced continuous flight times and prolonged resting times, other flight characteristics and navigational abilities showed no significant difference between infected and non-infected bees. Our results suggest that infected bees express normal flight characteristics but are constrained in their homing ability, potentially compromising the colony by reducing its resource inputs, but also counteracting the intra-colony spread of infection. We provide the first high-resolution analysis of sub-lethal effects of an emerging disease on insect flight behaviour. The potential causes and the implications for both host and parasite are discussed.
Ring-opening polymerizations (ROPs) of L-lactide are performed in bulk at 130°C with tin(II) 2-ethylhexanoate as catalyst and various phenols of differentacidity as initiators. Crystalline polylactides having phenyl ester end groups are isolated, which are almost free of cyclics. The dispersities and molecular weights are higher than those obtained from alcohol-initiated ROPs under identical conditions. Polymerizations at 160°C yield higher molecular weights than expected from the monomer/initiator ratio and a considerable fraction of cycles. The fraction of cycles increases with higher reactivity of the ester end group indicating that the cycles are formed by end-to-end cyclization.
Ring-opening polymerizations (ROP) of l-lactide (LA) are conducted in bulk at 130, 160, or 180 °C and are initiated with two different alcohols at 160 °C. The lactide/initiator ratio (LA/In) is varied from 50/1 (20/1 at 180 °C) to 900/1 and the lactide/catalyst ratio (LA/Cat) between 2000/1 and 8000/1. At all temperatures a nearly perfect control of number average molecular weight (Mn) via the LA/In ratio is feasible up to LA/In = 200/1, but at higher ratios the Mn value lags behind the theoretical values and the discrepancy increases with higher LA/Cat ratios. Variation of the LA/Cat ratio influences the formation of cycles but does not significantly influence Mn, when the LA/In ratio is kept constant. The formation of cycles is favored by lower In/Cat ratios and is the main reason for the unsatisfactory control of Mn at high LA/In ratios. The results also suggest that the cycles are mainly or exclusively formed by end-to-end cyclization and not, as believed previously, by back-biting.
Smart technical textiles are by definition textiles that can interact with their environment.
They can sense and react to environmental conditions and external stimuli from mechanical, thermal, chemical or other sources. Such textiles are multifunctional or even “intelligent” which is fulfilled by a number of sensors incorporated in the textiles. The embedded sensors are sensitive to various parameters such as temperature, strain, chemical, biological and other substances.
In civil engineering, many structures are made of reinforced concrete. Most Degradation processes relevant to this material, e.g., corrosion, are related to an increased level of material moisture.
Therefore, moisture monitoring in reinforced concrete is regarded as a crucial method for structural health monitoring. In this study, passive radio frequency identification (RFID)-based sensors are embedded into the concrete. They are well suited for long-term operation over decades and are well protected against harsh environmental conditions. The energy supply and the data transfer of the humidity sensors are provided by RFID. The sensor casing materials are optimised to withstand the high alkaline environment in concrete, having pH values of more than 12. Membrane materials are also investigated to identify materials capable of enabling water vapour transport from the porous cement matrix to the embedded humidity sensor. By measuring the corresponding relative humidity with embedded passive RFID-based sensors, the cement hydration is monitored for 170 days.
Moreover, long-term moisture monitoring is performed for more than 1000 days. The Experiments show that embedded passive RFID-based sensors are highly suitable for long-term structural health monitoring in civil engineering.
Smart Products Enable Smart Regulations—Optimal Durability Requirements Facilitated by the IoT
(2021)
The challenges and opportunities linked with IoT have been intensively discussed in recent years. The connectivity of things over their entire life cycle and the smart properties associated with it provide new functionalities and unprecedented availability of (usage) data. This offers huge opportunities for manufacturers, service providers, users, and also policymakers. The latter May impact policy areas such as the regulations on resource and materials efficiency under the Ecodesign Directive 2009/125/EC. With the general approach as it is practiced today, legal requirements are usually set for entire product groups without considering the products individually, including user behavior and environmental conditions. The increasing number of smart products and the growing availability of product data are sparking a discussion on whether these requirements could be more product and application-specific. This paper presents a method for calculating the economically and ecologically optimal durability of a product. It allows determining the point in time when a product should be replaced by combining consumer data with product design data. This novel Approach could contribute to making product regulation more flexible and possibly more efficient. In this context, fundamental challenges associated with smart products in policymaking are also discussed.
Increasing traffic volume on the one hand and ageing infrastructure on the other hand have created many new challenges for maintenance and structural health monitoring of roads and bridges. In the past, many bridges and road structures have been neglected, often resulting in traffic congestion, road closure, and increased repair costs.
This research is concerned with the development of a system to improve the challenge of maintenance and early detection of damage, particularly moisture penetration and corrosion of steel reinforced concrete components. The objective is to develop a method that will also work after 30 years and longer. Many new IoT solutions are equipped with internal energy storage elements (accumulators or batteries) which are inappropriate here, since most relevant signs of concrete degradation occur after decades, where the functioning of such elements are more than questionable. The presented technology approach uses radio-frequency identification (RFID) and enables connectivity to sensors. It offers the advantage of an passive, completely independent energy supply without any energy storage components.
Since the system should be permanently embedded in concrete, it is crucial to develop a long-term stable device which is adapted to the environmental influences of the structure, e.g., long-term resistance in very alkaline environment of pH 13. In numerous experiments, the robustness of the system was tested and evaluated. Various tests with encapsulations to protect the electronics were performed, and for long-term validation different concrete specimens were instrumented with RFID-sensor-systems. Their operating time is now around two years and investigations for signs of fatigue and damage to the encapsulation and the electronics are ongoing.
Increasing traffic volume on the one hand and ageing infrastructure on the other hand have created many new challenges for maintenance and structural health monitoring of roads and bridges. In the past, many bridges and road structures have been neglected, often resulting in traffic congestion, road closure, and increased repair costs.
This research is concerned with the development of a system to improve the challenge of maintenance and early detection of damage, particularly moisture penetration and corrosion of steel reinforced concrete components. The objective is to develop a method that will also work after 30 years and longer. Many new IoT solutions are equipped with internal energy storage elements (accumulators or batteries) which are inappropriate here, since most relevant signs of concrete degradation occur after decades, where the functioning of such elements are more than questionable. The presented technology approach uses radio-frequency identification (RFID) and enables connectivity to sensors. It offers the advantage of an passive, completely independent energy supply without any energy storage components.
Since the system should be permanently embedded in concrete, it is crucial to develop a long-term stable device which is adapted to the environmental influences of the structure, e.g., long-term resistance in very alkaline environment of pH 13. In numerous experiments, the robustness of the system was tested and evaluated. Various tests with encapsulations to protect the electronics were performed, and for long-term validation different concrete specimens were instrumented with RFID-sensor-systems. Their operating time is now around two years and investigations for signs of fatigue and damage to the encapsulation and the electronics are ongoing.
Evaluation of evacuation process is common separated by two phases: pre-movement and movement-phase. Individual capabilities of pedestrians have an impact on both and therefore on the time required for safe escape. In view of evaluating the evacuation process, characteristics of realistic movements of pedestrians involved are needed, but so far such data are mainly available for individuals with unrestricted evacuation capabilities only.
Due to the lack of available data, parameter studies in an assisted living for people with disabilities were performed to explore the movement during evacuation. Preparation times for assistance (n = 10), unimpeded walking speeds (n = 34) depending on the assistance devices in the plane as well as walking speeds on stairs (n = 11) were focussed.
Time to prepare an assistance device for utilisation depends significantly on the kind of device type. Further on, practical experience in handling the devices for assistance has an impact on the preparation time. In contrast to the results of the preparation times, any relation on assistance devices were investigated for the unimpeded walking speed in the plane. A remarkable decrease of walking speed on stairs was observed which is independent from the utilised assistance device.
The presented data improve and extend the insufficient engineering data base and raised up questions regarding the complexity of considering pedestrians movement with impairments in evacuation planning.
Functional fatigue of shape-memory alloys is a considerable threat to the reliable service of actuation devices. Here, we demonstrate the essentially degradation-free cyclic phase-transformation behavior of Ni-Mn-Ga microcrystals up to one million stress-driven superelastic cycles. Cyclic dissipation amounts to about 1/5 of the bulk counterpart and remains unaffected during cycling, even after the introduction of dislocation structures via plastic straining. Plastic yielding and the transformation stress largely exceed the known bulk values. However, the transformation-stress is found to depend on plastic pre-straining, which suggests that the size-affected transformation stress is sensitive to the initial defect structure and that it can be tuned by a targeted introduction of dislocations. These findings demonstrate the high suitability of Ni-Mn-Ga as a robust shape-memory alloy in small-scale functional device engineering.
A versatile software package in the form of a Python extension, named CDEF (computing Debye’s scattering formula for extraordinary form factors), is proposed to calculate approximate scattering profiles of arbitrarily shaped nanoparticles for small-angle X-ray scattering (SAXS). CDEF generates a quasi-randomly distributed point cloud in the desired particle shape and then applies the open-source software DEBYER for efficient evaluation of Debye’s scattering formula to calculate the SAXS pattern (https://github.com/j-from-b/CDEF). If self-correlation of the scattering signal is not omitted, the quasi-random distribution provides faster convergence compared with a true-random distribution of the scatterers, especially at higher momentum transfer. The usage of the software is demonstrated for the evaluation of scattering data of Au nanocubes with rounded edges, which were measured at the four-crystal monochromator beamline of PTB at the synchrotron radiation facility BESSY II in Berlin. The implementation is fast enough to run on a single desktop computer and perform model fits within minutes. The accuracy of the method was analyzed by comparison with analytically known form factors and verified with another implementation, the SPONGE, based on a similar principle with fewer approximations. Additionally, the SPONGE coupled to McSAS3 allows one to retrieve information on the uncertainty of the size distribution using a Monte Carlo uncertainty estimation algorithm.
Slicing - a new method for non destructive 3D elemental sensitive characterization of materials
(2014)
Recent advances in synchrotron sources and detector technology have led to substantial improvements in spatial resolution and detection limits for X-ray fluorescence analysis (XRF). However, the non-destructive three-dimensional elemental sensitive characterization of samples remains a challenge. We demonstrate the use of the so-called 'Color X-ray Camera' (CXC) for 3D measurements for the first time. The excitation of the sample is realized with a thin sheet-beam. The stepwise movement of the sample allows getting the elemental distribution for each layer with one measurement. These layers can be combined to a full 3D dataset for each element afterwards. Since the information is collected layer by layer, there is no need to apply reconstruction techniques, which quite often are the reason for artifacts in the results achieved by computed tomography (CT). The field of applications is wide, as the 3D elemental distribution of a material contains clues to processes inside the samples from a variety of origins. The technique is of special interest and well suited for biological specimens, because their light matrix minimizes restricting absorption effects. Measurement examples of a hornet and the teeth of a Sorex araneus are shown.
A facile and efficient methodology is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core–shell nanoparticles (NPs) for application in catalysis. The diameter of the NPs is tuned in a range from 6 nm to 30 nm and to adjust the Ni:Cu ratio from 30:1 to 1:1. Furthermore, the influence of different reaction parameters on the final NPs is studied. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Using these analytical methods, it is possible to elucidate a core–shell–shell structure of all particles and their chemical composition. In all cases, a depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core–shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction) independent of size and Ni:Cu ratio.