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Organisationseinheit der BAM
- 8 Zerstörungsfreie Prüfung (9)
- 8.5 Röntgenbildgebung (6)
- 1 Analytische Chemie; Referenzmaterialien (3)
- 6 Materialchemie (3)
- 6.1 Oberflächen- und Dünnschichtanalyse (3)
- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (3)
- 1.2 Biophotonik (2)
- 4 Material und Umwelt (2)
- 4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung (2)
- 5 Werkstofftechnik (2)
Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties.
Material extrusion of thermoplastic polymers enables the realization of complex specific designs with high performance composites. The present study aims at evaluating the mechanical properties of carbon fiberreinforced semi-crystalline thermoplastic polymer polyether ether ketone (CFR-PEEK) manufactured by material extrusion and correlating them with results obtained by micro-CT. Samples in the shape of small bars were provided by Kumovis (Munich, Germany). The determination of surface roughness and density was followed by three-point bending tests. To reveal the pore distribution as well as the fusion quality of CFR PEEK when applied with external forces, micro-CT scans were performed with an X-ray microscope before and after the mechanical test to localize the sites where the fracture is generated. The density of CFR-PEEK bars indicated that they had superior mechanical properties compared with our previous study on unfilled 3D printed PEEK (bending modulus: (5.4 ± 0.5) GPa vs. (1.05 ± 0.05) GPa to (1.48 ± 0.10) GPa; bending strength: (167 ± 11) MPa vs. (51 ± 15) to (193 ± 7) MPa). Micro-CT analyses revealed the local 3D-distribution of voids. Voids of 30 μm diameter are nearly spherical and make up the main part of the total porosity. The larger the voids, the more they deviate from a spherical shape. Significant lack-of-fusion voids are located between the deposited filaments. By growing and merging, they act as seeds for the forming fracture line in the region of the flexural specimens where the maximum local tensile stresses occurred under bending load. Our work provides a detailed analysis of printed PEEK with fiber additive and relates this with mechanical properties.
A combined theoretical and experimental investigation was carried out with the objective of evaluating theoretical predictions relating to a two-dimensional airfoil subjected to high amplitude harmonic oscillation of the free stream at constant angle of attack. Current theoretical approaches were reviewed and extended for the purposes of quantifying the bound, unsteady vortex sheet strength along the airfoil chord. This resulted in a closed form solution that is valid for arbitrary reduced frequencies and amplitudes. In the experiments, the bound, unsteady vortex strength of a symmetric 18 % thick airfoil at low angles of attack was measured in a dedicated unsteady wind tunnel at maximum reduced frequencies of 0.1 and at velocity oscillations less than or equal to 50 %. With the boundary layer tripped near the leading edge and mid-chord, the phase and amplitude variations of the lift coefficient corresponded reasonably well with the theory. Near the maximum lift coefficient overshoot, the data exhibited an additional high-frequency oscillation. Comparisons of the measured and predicted vortex sheet indicated the existence of a recirculation bubble upstream of the trailing edge which sheds into the wake and modifies the Kutta condition.
Without boundary layer tripping, a mid-chord bubble is present that strengthens during flow deceleration and its shedding produces a dramatically different effect.
Instead of a lift coefficient overshoot, as per the theory, the data exhibit a significant undershoot. This undershoot is also accompanied by high-frequency oscillations that are characterized by the bubble shedding. In summary, the location of bubble and ist subsequent shedding play decisive roles in the resulting temporal aerodynamic loads.
Objectives. There is concern that the integrity of fiberglass dental posts may be affected by chairside trimming during treatment. We hypothesize that hard X-ray methods of phase contrast-enhanced micro-CT (PCE-CT) and synchrotron based X-ray refraction (SXRR) can reliably identify and help characterize the extent of damage.
Methods. Fiberglass posts were imaged both as manufactured and following trimming with a diamond bur. Each of the posts was imaged by SXRR and by PCE-CT. Datasets from PCE-CT were used to visualize and quantify 2D and 3D morphological characteristics of intact and of damage-affected regions caused by trimming. Results. The SXRR images revealed fiber inhomogeneities from manufacturing with a significant increase in internal surfaces in sample regions corresponding to damage from trimming. PCE-CT volumes unveiled the micromorphology of single fibers in the posts and some damage in the trimmed area (e.g. fractures, splinters and cracks). Area, perimeter, circularity, roundness, volume and thickness of the glass fibers in the trimmed area were statistically different from the control (p < 0.01).
Significance. The integrity of single fibers in the post is critical for bending resistance and for long-term adhesion to the cement in the root canals. Damage to the fibers causes substantial structural weakening across the post diameter. Glass fragments produced due to contact with the dental bur may separate from the post and may significantly reduce bond capacity. The above mentioned synchrotron-based imaging techniques can further facilitate assessment of the structural integrity and the appearance of defects in posts (e.g. after mechanical load).
Determination of short carbon fiber orientation in zirconium diboride ceramic matrix composites
(2024)
In fiber-reinforced components, the fiber alignment and orientation have paramount influence on the thermomechanical properties of the resulting composite, for both short and continuous fiber. Here we present the case of an ultra-refractory matrix intended for extreme environment applications, ZrB2, reinforced with 20 vol% and 50 vol% short carbon fibers. In both cases, fibers tend to align perpendicular to the uniaxial pressure applied during shaping and sintering of a pellet, although the fiber tilt across the pellet thickness is difficult to determine. Moreover, for high volume fractions of reinforcement, the spatial distribution of the fibers is heterogeneous and tends to have domains of preferential orientations. We compare the information on the fiber distribution as collected by scanning electron microscopy images, X-ray computed tomography and synchrotron X-ray refraction radiography (SXRR). The three techniques prove to be complementary. Importantly, we demonstrate that SXRR yields the most statistically significant information due to the largest field of view, yet with a sensitivity down to the nanometer, and that can be successfully applied also to heavy matrix materials, such as zirconium boride.
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments.
In order to characterise the material and damage behaviour of additively manufactured polyamide 12 (PA12) under quasi-static load and to implement it in a numerical model, experiments under quasi-static load as well as microstructural investigations were carried out. Selective laser sintering (SLS) was used as the manufacturing process. For the classification of the material behaviour, quasi-static cyclic tests with holding times as well as tensile tests were performed. X-ray refraction and computed tomography (CT) were used to investigate the damage behaviour. The Chaboche model, which has already been applied for metallic materials under thermomechanical loading, served as the basis for the selection of the numerical material model. The same procedure was used for the selection of the damage model, where the Gurson–Tvergaard–Needleman (GTN) model was chosen, which was already used for porous metallic materials. The Chaboche model shows very good agreement with experimental results. Furthermore, the coupling with the GTN model allows a very good modelling of the damage behaviour. Finally, it could be shown that the selected models are suitable to simulate the material and damage behaviour of 3D printed PA12.
We measured and collected literature data for the crystal growth rate, u(T), of µ-cordierite (2MgO · 2Al2O3 · 5SiO2) and diopside (CaO · MgO · 2SiO2) in their isochemical glass forming melts. The data cover exceptionally wide temperature ranges, i.e. 8001350 °C for cordierite and 7501378 °C for diopside. The maximum of u(T) occurs at about 1250 °C for both systems. A smooth shoulder is observed around 970 °C for µ-cordierite. Based on measured and collected viscosity data, we fitted u(T) using standard crystal growth models. For diopside, the experimental u(T) fits well to the 2D surface nucleation model and also to the screw dislocation growth mechanism. However, the screw dislocation model yields parameters of more significant physical meaning. For cordierite, these two models also describe the experimental growth rates. However, the best fittings of u(T) including the observed shoulder, were attained for a combined mechanism, assuming that the melt/crystal interface growing from screw dislocations is additionally roughened by superimposed 2D surface nucleation at large undercoolings, starting at a temperature around the shoulder. The good fittings indicate that viscosity can be used to assess the transport mechanism that determines crystal growth in these two systems, from the melting point Tm down to about Tg, with no sign of a breakdown of the StokesEinstein/Eyring equation.
A major industrial reaction based on homogeneous catalysis is hydroformylation for the production of aldehydes from alkenes and syngas. Hydroformylation in microemulsions, which is currently under investigation at Technische Universität Berlin on a mini-plant scale, was identified as a cost efficient approach which also enhances product selectivity. Herein, we present the application of online Raman spectroscopy on the reaction of 1-dodecene to 1-tridecanal within a microemulsion. To achieve a good representation of the operation range in the mini-plant with regard to concentrations of the reactants a design of experiments was used. Based on initial Raman spectra partial least squares regression (PLSR) models were calibrated for the prediction of 1-dodecene and 1-tridecanal. Limits of predictions arise from nonlinear correlations between Raman intensity and mass fractions of compounds in the microemulsion system. Furthermore, the prediction power of PLSR models becomes limited due to unexpected by-product formation. Application of the lab-scale derived calibration spectra and PLSR models on online spectra from a mini-plant operation yielded promising estimations of 1-tridecanal and acceptable predictions of 1-dodecene mass fractions suggesting Raman spectroscopy as a suitable technique for process analytics in microemulsions.
Dynamic stall often occurs under conditions of simultaneous unsteady pitching and surging (e.g., rotorcraft and wind turbines), butmanymodels employ a dimensionless time base that implicitly assumes that surging is superimposed, in a quasi-steady manner, on dynamic pitching. An unsteady wind tunnel was used to examine this assumption, where a technique was developed to quantify the unsteady effects of surging on a pitching NACA 0018 airfoil. The technique involved performing multiple harmonic pitching experiments under nominally steady freestream conditions that bracketed a corresponding 50% surging amplitude (1.25 ⋅ 105 ≤ Re ≤ 3.75 ⋅ 105). By interpolating these data, unsteady-pitching/quasi-steady-surging data sets were constructed and compared with de facto synchronous pitch and surging experiments, thereby isolating the unsteady effects of surging on a pitching airfoil. Both large and small poststall maximum angles of attack (αs + 5° and αs + 15°) were considered at multiple pitch-surge phase differences. During deep dynamic stall (αs 15°), with large-scale separation, surging was seen to have a secondary effect on the unsteady aerodynamics. However, at small poststall maximum angles of attack (αs + 5°), either light or deep dynamic stall behavior was observed depending upon the pitch-surge phase difference. This was attributed to Reynolds number history effects, exemplified by boundary-layer transition, and thus it can be referred to as “transitional” dynamic stall.
Ingenieurbauten des Bundesfernstraßenbereichs sind aufgrund ihrer Exposition an vielen Stellen besonders betroffen von Graffiti. Graffitischmierer nehmen hierbei keine Rücksicht auf die Art der Substratmaterialien, und besonders poröse Untergründe bereiten Schwierigkeiten bei der Reinigung. Um Baustoffoberflächen besser zu schützen und von Graffiti leichter reinigen zu können, wurden in den vergangen Jahren spezielle Prophylaxesysteme (Anti-Graffiti-Systeme, AGS) entwickelten. Für die Beurteilung der Funktionalität und Verwendbarkeit dieser Anti-Graffiti-Systeme wurden von der Bundesanstalt für Straßenwesen (BASt) eine neue Technische Prüfvorschrift und Technische Lieferbedingungen (TP/TL AGS-Beton) erarbeitet. Die TP/TL AGS-Beton gilt hierbei nur für die Beurteilung von AGS auf Betonuntergründen. In einer Forschungsstudie wurde untersucht, inwieweit die vorhandene Prüfvorschrift für Betonsubstrate auch auf andere Untergründe, z. B. Naturstein oder Klinker, angewendet werden kann. Weiterhin wurde untersucht, welche Faktoren eine Rolle bei der Reinigung von mit AGS behandelten verschiedenen Substraten spielen.
We propose a model to describe the sintering kinetics of polydispersed glass particles, having no adjustable parameter. The model is based on three sintering stages: a pure Frenkel' (F) first step, a mixed Frenkel/MackenzieShuttleworth' stage, and a third, pure MackenzieShuttleworth' (MS) step. The model considers sample shrinkage as the sum of the partial shrinkage of several clusters, each consisting of equally sized particles and each showing independent F or MS behavior. The overall set of clusters mimics the specimen's real particle size distribution. We then introduce the concept of neck forming ability, which allows the formation of necks among particles of different sizes, relaxing the clustering condition. Using experimental physical parameters: particle size distribution, viscosity, surface energy, and the theoretical neck forming ability, the model describes well the sintering kinetics of an alumino-borosilicate glass powder having polydispersed, irregular shaped particles in a variety of temperatures. The sintering kinetics of the real powder is slower, but not far from the calculated kinetics of a monodispersed distribution containing only particles of average size. Thus the model provides a tool for estimating the sintering kinetics of real glass powders, for any size distribution and temperature, thus minimizing the number of laboratory experiments.
Gated detection with intensified detectors, e.g., ICCDs, is today the accepted approach for detection of plasma emission in laser-induced breakdown spectroscopy (LIBS). However, these systems are more cost-intensive and less robust than nonintensified CCDs. The objective of this paper is to compare, both theoretically and experimentally, the performance of an intensified (ICCD) and nonintensified (CCD) detectors for detection of plasma emission in LIBS. The CCD is used in combination with a mechanical chopper, which blocks the early continuum radiation from the plasma. The detectors are attached sequentially to an echelle spectrometer under the same experimental conditions. The laser plasma is induced on a series of steel samples under atmospheric conditions. Our results indicate that there is no substantial difference in the performance of the CCD and ICCD. Signal-to-noise ratios and limits of detection achieved with the CCD for Si, Ni, Cr, Mo, Cu, and V in steel are comparable or even better than those obtained with the ICCD. This result is further confirmed by simulation of the plasma emission signal and the corresponding response of the detectors in the limit of quantum (photon) noise.
Because the demining process is always connected with a danger for human beings, it is necessary to make sure the proper functioning of mine searching equipment in detecting mines. Detecting a hidden target by penetrating physical interaction of rays or waves is similar to non-destructive testing. The non-destructive testing profession developed procedures to check the reliability of testing. These procedures, like the performance demonstration where the successful detections are statistically evaluated against false call rates and their implementation in an industrial standard (ASME section XI appendix VIII) are used as a template. A first adoption to demining was accomplished in the prescription for blind trials in the CEN workshop agreement CWA 14747: 2003 for test and evaluation of metal detectors. Within an ITEP project a number of blind trials were carried out to learn about the necessary statistical basis of those trials to achieve true, reproducible and repeatable results to give guidance for the selection and improvement of metal detectors. The special focus in this first investigation was on the influence of the human factor due to the different degree of experience of the operators and the influence of the soil.
The total reliability of a mine searching system is driven by the triple of intrinsic
capability, which describes the physical-technical basis capability, the application and
environmental factors and the human factors. Some of them can be determined in
laboratory measurements but the human factor and a part of environment conditions
and their interaction with the device need to be treated statistically. That is why the
test & evaluation procedure described in CEN CWA 14747:2003, includes in addition
to parameter tests of metal detectors also the reliability or blind field tests under local
conditions with local personnel. A series of three big field trials had been
accomplished in the ITEP-project 2.1.1.2 Reliability Model for Test & Evaluation of
Metal Detectors to specify the optimum conditions for reliable trial results with
affordable effort. For each set of specific working conditions, characterized in terms
of a combination of one mine type in one soil with one detector handled by local
personnel, the searching system will show up a working performance in mine
detection rates as a function of mine depth and show up a certain overall false call
rate. During the ITEP-trials in Benkovac and Oberjettenberg the authors learnt to
determine this function separately for each mine type in each soil, which is especially
important for low metal mines in uncooperative soil which will be illustrated for the
mine PMA2 in different types of soil. The question of representativeness for field
conditions on the one hand and necessary statistical set up for the possibility to
distinguish between individual detector performances is still under discussion.
Die Bewertung von VOC-Emissionen aus Bauprodukten soll durch das AgBB-Schema vereinheitlicht werden und eine gesundheitsrelevante Komponente enthalten. Das Deutsche Institut für Bautechnik (DIBt) hat das AgBB-Schema in weiten Teilen für seine Grundsätze zur gesundheitlichen Bewertung von Bauprodukten in Innenräumen implementiert. Neben der üblichen chemischen Emissionsmessung soll auch der Geruch für die Bewertung des Produkts herangezogen werden. Um den Geruch als festen Bestandteil in die Produktprüfung zu integrieren, wurden vom Umweltbundesamt zwei Vorhaben initiiert. Erste Ergebnisse des zweiten Vorhabens (FKZ 37 07 62 300; Sensorische Bewertung der Emissionen aus Bauprodukten Integration in die Vergabegrundlagen für den Blauen Engel und das Bewertungsschema des Ausschusses zur gesundheitlichen Bewertung von Bauprodukten) werden hier dargestellt.
Um eine gute Luftqualität in Gebäuden zu erreichen, müssen Reinigungslasten durch Lüften aus Räumen abgeführt bzw. vermieden oder verringert werden. Wird der Luftwechsel verringert, verschlechtert sich die Raumluftqualität, und die Zufriedenheit der Nutzer nimmt ab. An Arbeitsplätzen kann es bei schlechter Luftqualität und der daraus resultierenden Unzufriedenheit zu einer geringeren Produktivität der Beschäftigten kommen. Um die Reinigungslasten und deren Wirkung auf den Raumnutzer überdas Geruchsempfinden zu verringern, ist neben einer messtechnischen Erfassung der Verunreinigungen auch eine sensorische Prüfung in Innenräumen und von Bauprodukten notwendig. In diesem Artikel wird die Entwicklung der Bewertungsmethodik von Gerüchen im Innenraum erläutert und auf Anwendungen eingegangen.