Ingenieurwissenschaften und zugeordnete Tätigkeiten
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CONRAD-2 is an imaging instrument using low-energy (cold) neutrons. The instrument is installed at the end of a curved neutron guide which avoids the direct line of sight towards the reactor core. This ensures a very low background of high-energy neutrons and. photons at the sample position. The cold neutron beam provides a wavelength range which is suitable for phase-and diffraction-contrast imaging such as grating interferometry and Bragg edge mapping. The instrument is well suited for high resolution imaging due to the high efficiency of the very thin scintillators that can be used for the detection of cold neutrons. An instrument upgrade was performed recently as a part of an upgrade program for the cold neutron instrumentation at HZB. The parameters of the instrument as well as some research highlights will be presented.
Many industrial processes are run at non-atmospheric conditions (elevated temperatures and pressures, other oxidizers than air). To judge whether and if yes to what extent explosive gas(vapor)/air mixtures will occur or may be generated during malfunction it is necessary to know the safety characteristic data at the respective conditions. Safety characteristic data like Explosion limits, are depending on pressure, temperature and the oxidizer. Most of the determination methods are standardized for ambient conditions.
In order to obtain determination methods for non-atmospheric conditions, particularly for higher initial pressures, reliable ignition criteria were investigated. Ignition tests at the explosion Limits were carried out for mixtures of methane, propane, n-butane, n-hexane, hydrogen, ammonia and acetone in air at initial pressures up to 20 bar. The tests have been evaluated according to different ignition criteria: visual flame propagation, temperature and pressure rising. It could be shown that flame propagation and occasionally self-sustained combustion for several seconds occurred together with remarkable temperature rise, although the pressure rise was below 3%. The results showed that the combination of a pressure rise criterion of 2% and a temperature rise criterion of 100 K seems to be a suitable ignition criterion for the determination of explosion limits and limiting oxidizer concentration at higher initial pressures and elevated temperatures. The tests were carried out within the framework of a R&D project founded by the German Ministry of Economics and Technology.
In this paper we present results of our recent efforts to understand the mechanical interface behaviour of single-walled carbon nanotubes (CNTs) embedded in metal matrices. We conducted experimental pull-out tests of CNTs embedded in Pd or Au and found Maximum forces in the range 10 - 102 nN. These values are in good agreement with forces obtained from molecular Dynamics simulations taking into account surface functional Groups (SFGs) covalently linked to the CNT material. The dominant failure mode in experiment is a CNT rupture, which can be explained with the presence of SFGs. To qualify the existence of SFGs on our used CNT material, we pursue investigations by means of fluorescence labeling of surface species in combination with Raman imaging. We also report of a tensile test system to perform pull-out tests inside a transmission electron microscope to obtain in situ images of CNT-metal interfaces under mechanical loads at the atomic scale.
Melt flow and dripping of the pyrolysing polymer melt can be both a benefit and a detriment during a fire. In several small-scale fire tests addressing the ignition of a defined specimen with a small ignition source, well-adjusted melt flow and dripping are usually beneficial to pass the test. The presence of flame retardants often changes the melt viscosity crucially. The influence of certain flame retardants on the dripping behaviour of four commercial polymers, poly(butylene terephthalate) (PBT), polypropylene (PP), polypropylene modified with ethylene-propylene rubber (PP-EP) and polyamide 6 (PA 6), is analysed based on an experimental monitoring of the mass loss due to melt dripping, drop size and drop temperature as a function of the furnace temperature applied to a rod-shaped specimen. Investigating the thermal transition (DSC), thermal and thermo-oxidative decomposition, as well as the viscosity of the polymer and collected drops completes the investigation. Different mechanisms of the flame retardants are associated with their influence on the dripping behaviour in the UL 94 test. Reduction in decomposition temperature and changed viscosity play a major role. A flow limit in flame-retarded PBT, enhanced decomposition of flame-retarded PP and PP-EP and the promotion of dripping in PA 6 are the salient features discussed.
A user-friendly open-source Monte Carlo regression package (McSAS) is presented, which structures the analysis of small-angle scattering (SAS) using uncorrelated shape-similar particles (or scattering contributions). The underdetermined problem is solvable, provided that sufficient external information is available. Based on this, the user picks a scatterer contribution model (or 'shape') from a comprehensive library and defines variation intervals of its model parameters. A multitude of scattering contribution models are included, including prolate and oblate nanoparticles, core-shell objects, several polymer models, and a model for densely packed spheres. Most importantly, the form-free Monte Carlo nature of McSAS means it is not necessary to provide further restrictions on the mathematical form of the parameter distribution; without prior knowledge, McSAS is able to extract complex multimodal or odd-shaped parameter distributions from SAS data. When provided with data on an absolute scale with reasonable uncertainty estimates, the software outputs model parameter distributions in absolute volume fraction, and provides the modes of the distribution (e.g. mean, variance etc.). In addition to facilitating the evaluation of (series of) SAS curves, McSAS also helps in assessing the significance of the results through the addition of uncertainty estimates to the result. The McSAS software can be integrated as part of an automated reduction and analysis procedure in laboratory instruments or at synchrotron beamlines.
SASfit: a tool for small-angle scattering data analysis using a library of analytical expressions
(2015)
SASfit is one of the mature programs for small-angle scattering data analysis and has been available for many years. This article describes the basic data processing and analysis workflow along with recent developments in the SASfit program package (version 0.94.6). They include (i) advanced algorithms for reduction of oversampled data sets, (ii) improved confidence assessment in the optimized model parameters and (iii) a flexible plug-in system for custom user-provided models. A scattering function of a mass fractal model of branched polymers in solution is provided as an example for implementing a plug-in. The new SASfit release is available for major platforms such as Windows, Linux and MacOS. To facilitate usage, it includes comprehensive indexed documentation as well as a web-based wiki for peer collaboration and online videos demonstrating basic usage. The use of SASfit is illustrated by interpretation of the small-angle X-ray scattering curves of monomodal gold nanoparticles (NIST reference material 8011) and bimodal silica nanoparticles (EU reference material ERM-FD-102).
Simple models describing the relationship between basic mechanical properties and the relative density of various types of porous metals (such as foams, sponges and lattice structures) are well established. Carefully evaluating these relationships experimentally is challenging, however, because of the stochastic structure of foams and the fact that it is difficult to systematically isolate density changes from variations in other factors, such as pore size and pore distribution. Here a new method for producing systematic sets of stochastic foams is employed based on electron beam melting (EBM) additive manufacturing (AM). To create idealised structures, structural blueprints were reverse-engineered by inverting X-ray computed tomographs of a randomly packed bed of glass beads. This three-dimensional structure was then modified by computer to create five foams of different relative density ρr, but otherwise consistent structure. Yield strength and Young’s modulus have been evaluated in compression tests and compared to existing models for foams. A power of 3 rather than a squared dependence of stiffness on relative density is found, which agrees with a recent model derived for replicated foams. A similar power of 3 relation was found for yield strength. Further analysis of the strength of nominally fully dense rods of different diameters built by EBM AM suggest that surface defects mean that the minimum size of features that can be created by EBM with similar strengths to machined samples is ∼1 mm.
Microorganisms accumulate molar concentrations of compatible solutes like ectoine to prevent proteins from denaturation. Direct structural or spectroscopic information on the mechanism and about the hydration shell around ectoine are scarce. We combined surface plasmon resonance (SPR), confocal Raman spectroscopy, molecular dynamics simulations, and density functional theory (DFT) calculations to study the local hydration shell around ectoine and its influence on the binding of a gene-S-protein (G5P) to a single-stranded DNA (dT(25)). Due to the very high hygroscopicity of ectoine, it was possible to analyze the highly stable hydration shell by confocal Raman spectroscopy. Corresponding molecular dynamics simulation results revealed a significant change of the water dielectric constant in the presence of a high molar ectoine concentration as compared to pure water. The SPR data showed that the amount of protein bound to DNA decreases in the presence of ectoine, and hence, the protein-DNA dissociation constant increases in a concentration-dependent manner. Concomitantly, the Raman spectra in terms of the amide I region revealed large changes in the protein secondary structure. Our results indicate that ectoine strongly affects the molecular recognition between the protein and the oligonudeotide, which has important consequences for osmotic regulation mechanisms.
A new method for sampling wear particles directly from the lubricant reservoir has been developed and applied successfully for analyzing wear particles by high-resolution scanning electron microscopy in transmission mode having coupled energy-dispersive X-ray spectroscopy. The lubricated tribological testing was carried out with fully formulated as well as with non-formulated synthetic base oil. It was possible to analyze individual particles with dimensions as small as about 5–30 nm which are likely the 'primary' wear particles. A majority of the particles, however, are agglomerated and, thus, lead to the formation of larger agglomerates of up to a few micrometers. Chemical analysis led to the conclusion that most of the observed particles generated in formulated oil, especially the larger ones, are composed of the additives of the lubricant oil. In non-formulated base oil, the primary particles are of similar dimensions but contain only iron, chromium and oxygen, but most likely stem from the mating materials. This finding points to the fact that the main wear mechanism under lubricated conditions with fully formulated oil is more like a continuous shearing process rather than a catastrophic failure with the generation of larger primary particles. When the oil is non-formulated, however, several wear mechanisms act simultaneously and the wear rate is increased significantly. Generated larger primary particles are milled down to the nanoscale. When the oil is fully formulated, wear mainly takes places at the additive layer or tribofilm; thus, the steel surface is protected.
Selective Electron Beam Melting (SEBM) is a promising powder bed Additive Manufacturing technique for near-net-shape manufacture of high-value titanium components. However without post-manufacture HIPing the fatigue life of SEBM parts is currently dominated by the presence of porosity. In this study, the size, volume fraction, and spatial distribution of the pores in model samples have been characterised in 3D, using X-ray Computed Tomography, and correlated to the process variables. The average volume fraction of the pores (b0.2%) was measured to be lower than that usually observed in competing processes, such as selective laser melting, but a strong relationship was found with the differentbeamstrategies used to contour ,and infill by hatching, a part section. The majority of pores were found to be small spherical gas pores, concentrated in the infill hatched region; this was attributed to the lower energy density and less focused beam used in the infill strategy allowing less opportunity for gas bubbles to escape the melt pool. Overall, increasing the energy density or focus of the beam was found to correlate strongly to a reduction in the level of gas porosity. Rarer irregular shaped pores were mostly located in the contour region and have been attributed to a lack of fusion between powder particles.