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Paper des Monats
- ja (68)
The color X-ray camera SLcam® is a full-field, single photon detector providing scanning-free, energy and spatially resolved X-ray imaging. Spatial resolution is achieved with the use of polycapillary optics guiding X-ray photons from small regions on a sample to distinct energy dispersive pixels on a charged-coupled device detector. Applying sub-pixel resolution, signals from individual capillary channels can be distinguished. Therefore, the SLcam® spatial resolution, which is normally limited to the pixel size of the charge-coupled device, can be improved to the size of individual polycapillary channels. In this work a new approach to a sub-pixel resolution algorithm comprising photon events also from the pixel centers is proposed. The details of the employed numerical method and several sub-pixel resolution examples are presented and 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.
Fire and explosion hazards associated with storage and transportation of flammable materials have been a matter of great interest in the recent times. BLEVE is a scenario that occurs when a closed fuel container is subjected to heat for a longer duration. Such events are disastrous to human beings and assets both. In the past there have been numerous studies on BLEVEs and fireballs of hydrocarbon fuels, e.g. kerosene, gasoline, LPG, LNG and others. Though, the fireballs of peroxy-fuels are not looked into detail as such. This article tries to overcome this lack of knowledge. Both, experimental investigation and CFD simulations are performed to measure and predict the fireball characteristics of a peroxy-fuel. Due to thermal decomposition in the liquid phase and active oxygen content a peroxy-fuel fireball burns at a very fast rate and emit higher thermal radiation whereas exhibits smaller diameter and elevation compared to hydrocarbons. That eventually leads to consideration of larger safety distances from them which are also verified by CFD results.
Temperature-memory polymers are able to generate a substantial mechanical response when heated above the temperature, at which a preceding deformation was carried out. Here we show how to design the temperature-memory effect (TME) by thermomechanical treatment. As a model polymer, phase segregated poly(ester urethane) (PEU) containing crystallizable segments of poly(1,4-butylene adipate) (PBA) was used. For programming, strain elongation was applied at temperatures within the PBA melting transition area, before temperature holding, unloading and cooling were carried out. Upon heating under stress-free or constant strain recovery conditions, precisely set temperature-memory onsets could be witnessed. Most importantly, strain fixities and recoverabilities the same as maximum recovery stresses turned out to be controllable by strain rate and temperature holding time after deformation, while transition temperatures remained largely unaffected. The tailoring of thermoresponsiveness was structurally enabled by different PBA crystallinities in the programmed state as verified by wide-angle X-ray scattering (WAXS). The reported studies intend to design TMEs in semicrystalline polyurethanes according to user-defined needs to make this technology broadly applicable.
Für die Durchführung einer Dichtheitsprüfung und für die Bewertung des Ergebnisses ist es wichtig, den sich unter Betriebsbedingungen im Prüfobjekt einstellenden Überdruck zu kennen. Entspricht der Prüfüberdruck nicht dem Betriebsüberdruck, so ist es oft erforderlich, die unter Prüfbedingungen gemessenen Leckageraten auf den realen Betriebsüberdruck umzurechnen. Im Bereich der Gefahrgutverpackungen ist jedoch der spätere maximale Betriebsüberdruck nicht genau bekannt. Er hängt für jede einzelne Verpackungsbauart von dem eingefüllten Füllmedium mit seinen spezifischen Stoffeigenschaften, dem Füllgrad sowie den Beförderungsbedingungen, insbesondere der mittleren Transporttemperatur, ab. Es werden Berechnungsansätze vorgestellt, mit denen sich der Überdruck in Gefahrgutverpackungen unter Beförderungsbedingungen rechnerisch ermitteln lässt. Die theoretisch berechneten Überdrücke werden mit Überdruck-Messwerten verglichen, die mit verschiedenen Füllmedien in unterschiedlichen Verpackungsbauarten ermittelt wurden.
Geosynthetics are planar polymeric products, which are used in connection with soil, rock or other soil-like materials to fulfill various functions in geoenvironmental engineering. Geosynthetics are of ever-growing importance in the construction industry. Sealing of waste storage facilities to safely prevent the emission of wastewater, landfill gas and contaminated dust as well as the diffusion of pollutants into the environment and coastal protection against storms and floods and reconstruction after natural disaster are important fields of application. We will give an overview of the various geosynthetic products. Two examples of the material problems related to geosynthetics are discussed in detail: the effect of creep on the long-term performance of geocomposite drains and the numerical simulation of the interaction of soil with geogrids. Both issues are of importance for the use of these products in landfill capping systems. The various functions, which geosynthetics may fulfill in the protection of coastal lines, are illustrated by case studies. The geosynthetic market is evaluated and economical and environmental benefits, as well as environmental side effects related to the use of geosynthetics, are discussed.
Durch den Einsatz von faserverstärkten Kunststoffen und Multi-Material-Konstruktionen zur Gewichtsreduzierung erlangen Klebeverbindungen immer stärkere Bedeutung. Die Prüfung dieser Fügeverbindungen stellt neue Anforderungen an die zerstörungsfreie Prüfung. Hinzu kommt, dass die Zugänglichkeit häufig eingeschränkt und die Verwendung flüssiger Koppelmittel aufgrund konstruktiver oder fertigungstechnischer Gegebenheiten ausgeschlossen ist. Unter Berücksichtigung dieser Beschränkungen wurde ein Prüfverfahren entwickelt, das eine luftgekoppelte Anregung geführter Ultraschallwellen mit einer laserbasierten Detektion kombiniert. Nachdem das Prüfverfahren zunächst mit einer einfachen Signalauswertung im Zeitbereich getestet wurde, konnte in nachfolgenden Untersuchungen die örtliche Auflösung durch die Implementierung von Filteralgorithmen im Frequenz-Wellenzahl-Bereich und zusätzlich durch direktionale Filter erhöht werden. Das resultierende bildgebende Prüfverfahren wurde an realitätsnahen Klebeproben mit künstlichen Fehlern getestet. Die Zuverlässigkeit und Ortsauflösung des Verfahrens wurde im Vergleich mit herkömmlichen Prüfverfahren validiert. Mithilfe des Verfahrens können Poren, Einschlüsse und Bereiche mit ungenügender Verklebung detektiert werden.
Online-Strukturüberwachungssysteme sind eine Möglichkeit, den Anforderungen hinsichtlich Leichtbau und Zuverlässigkeit gleichzeitig gerecht zu werden. Die Integration solcher Systeme liefert aktuelle Informationen über die Integrität der sicherheitsrelevanten Struktur, wodurch sich Aussagen über notwendige Instandhaltungsarbeiten und möglicherweise über die zu erwartende Restlebensdauer ableiten lassen. Der zielgerichtete Einsatz der Überwachungssysteme ermöglicht es somit, die benötigten Sicherheitsfaktoren bei der Auslegung der Bauteile zu reduzieren und Wartungsintervalle zu verlängern. Dadurch können Kosten gesenkt werden, ohne die Zuverlässigkeit zu verringern. Im Rahmen einer Studie zur Machbarkeit eines Online-Überwachungssystems für Eisenbahn-Radsatzwellen wurde der Einsatz geführter Ultraschallwellen, die von Sensoren an einer Stirnseite der Wellen angeregt werden, demonstriert. Aufgrund der Bauteilgeometrie und der dispersiven, multimodalen Wellenausbreitung stellt die Interpretation der Echosignale eine wesentliche Herausforderung dar. Basierend auf dem a-priori-Wissen über die Wellenausbreitung wurden in der Studie klassifizierende Auswertealgorithmen entwickelt und erfolgreich an maßstabsgetreuen Labormodellen getestet.
Hochduktiler Beton eröffnet neue Möglichkeiten bei der Instandsetzung von Bauwerken, der Herstellung dünnwandiger Bauelemente oder dem Einsatz von Dämpfungselementen in stoßartig beanspruchten Bauwerken (z.B. in Erdbebengebieten).
Die Steigerung der Duktilität kann durch die Zugabe von Kurzfasern erreicht werden. Im Falle einer Rissbildung in der Zementsteinmatrix überbrücken die Fasern den Riss, nehmen die Spannung vollständig auf und stoppen lokal das Risswachstum. Bei weiterer Steigerung der Last reißt die Matrix an anderer Stelle. Auf diese Weise wird die Rissbildung fein verteilt und es werden große Dehnungen erreicht, bevor das Bauteil versagt. Zur Optimierung der Festbetoneigenschaften müssen die Matrixfestigkeit und die Faserart sowie deren Gehalt aufeinander abgestimmt werden. Dabei sind auch die Verarbeitungseigenschaften des Frischbetons zu berücksichtigen.
Anhand der Schallemissionen kann die Rissbildung in der Matrix und die Interaktion mit den Fasern analysiert werden. So konnte in ersten Zugversuchen gezeigt werden, dass sich Schallereignisse dem Versagen der Zementsteinmatrix bzw. dem Auszug der Fasern aus der Matrix zuordnen lassen. Damit steht zur Beurteilung des mechanischen Verhaltens von hochduktilem Beton neben der Spannungs-Dehnungs-Linie ein weiteres Verfahren zur Verfügung.
Quantifying degradation of collagen in ancient manuscripts: the case of the Dead Sea Temple Scroll
(2013)
Since their discovery in the late 1940s, the Dead Sea Scrolls, some 900 ancient Jewish texts, have never stopped attracting the attention of scholars and the broad public alike, because they were created towards the end of the Second Temple period and the 'time of Christ'. Most of the work on them has been dedicated to the information contained in the scrolls' text, leaving physical aspects of the writing materials unexamined. They are, however, crucial for both historical insight and preservation of the scrolls. Although scientific analysis requires handling, it is essential to establish the state of degradation of these valued documents. Polarized Raman Spectroscopy (PRS) is a powerful tool for obtaining information on both the composition and the level of disorder of molecular units. In this study, we developed a non-invasive and non-destructive methodology that allows a quantification of the disorder (that can be related to the degradation) of protein molecular units in collagen fibers. Not restricted to collagen, this method can be applied also to other protein-based fibrous materials such as ancient silk, wool or hair. We used PRS to quantify the degradation of the collagen fibers in a number of fragments of the Temple Scroll (11Q19a). We found that collagen fibers degrade heterogeneously, with the ones on the surface more degraded than those in the core.
Synthesis, structure determination, and formation of a theobromine: oxalic acid 2:1 cocrystal
(2015)
The structure and the formation pathway of a new theobromine : oxalic acid (2 : 1) cocrystal are presented. The cocrystal was synthesised mechanochemically and its structure was solved based on the powder X-ray data. The mechanochemical synthesis of this model compound was studied in situ using synchrotron XRD. Based on the XRD data details of the formation mechanism were obtained. The formation can be described as a self-accelerated ('liquid like') process from a highly activated species.
Klebverbindungen im modernen Hochbau können helfen, innovative ästhetische Bedürfnisse im Fassadenbau umzusetzen, technologische Verbesserungen zu erreichen, aber auch die Wechselwirkung von Gebäuden mit der Umwelt unter energetischen Aspekten zu optimieren. Aufgrund der hohen sicherheitstechnischen Bedeutung gibt es hohe Anforderungen an die Leistungsfähigkeit, Dauerhaftigkeit und die Gütesicherheit.
Mit einer zerstörungsfreien praxistauglichen Prüftechnik, die eine sichere Überprüfung der Integrität von Glas-Metall Klebverbindungen im Ingenieurhochbau gewährleistet, kann sowohl ein wichtiger Beitrag zur Qualitätssicherung bei der Herstellung von Fassadenelementen aber auch bei der späteren Bauwerksüberwachung im Verlauf der Nutzungsdauer geleistet werden. Für eine Beurteilung der Qualität der Verbundfuge (z.B. bezgl. Standsicherheit) sind dabei Aussagen zur Homogenität der Verbundfuge, zum adhäsiven und kohäsiven Verbundverhalten gefordert. Hierzu besteht aktuell insbesondere Bedarf an zerstörungsfreien praxisgerechten, hoch ortsauflösenden und möglichst bildgebenden Untersuchungsverfahren.
Es wird mit einem Matrixarray und mit konventionellen Winkelprüfköpfen eine Prüftechnik vorgestellt, mit der die Wechselwirkung zwischen Ultraschallwelle und Fehlstelle in der Klebefuge untersucht wird. Hierbei ist das erste Untersuchungsziel, mit einer angepassten Ultraschall-Prüftechnik mögliche Inhomogenitäten oder Schädigungsstellen in der geklebten Glas-Metall Verbindung zu detektieren.
Über diese qualitativen Aussagen hinaus werden weiterführende Informationen über die flächenhafte Ausdehnung und den Ort einer mangelnden Klebung ermittelt. Dazu werden die Messwerte zusammen mit den Positionen des Ultraschallprüfkopfs aufgezeichnet. Mit Hilfe einer bildhaften Auswertung der gemessenen Ultraschallechos in Abhängigkeit vom Prüfkopfort werden die Möglichkeiten einer detaillierten Integritätsanalyse der Glas-Metall Klebschicht dargestellt. In diesem Beitrag werden experimentelle Prüfergebnisse vorgestellt, die im Sinne einer Verfahrensvalidierung an einem speziellen Beispielprobekörper zur Nachstellung einer SSG-Verglasung (ermittelt wurden und die Detektion fehlerhafter Klebestellen in einer Glas-Metall-Klebverbindung zum Ziel haben.
The objective of the report is to present the state-of-the art of non-destructive testing methods and technologies for the inspection of thick, heavily-reinforced structures, (e.g. found in nuclear power plants). Wall thicknesses can be in excess of one meter and the structures often have increased steel reinforcement density. The accessibility for any testing method may be limited due to the presence of liners and other components such as cast-in-place items. Testing methods have to provide solutions for tasks such as locating failure (inclusions, corrosion, voids, delaminations) in the structures or the assessment of the condition of the structure in general.
Solgel prepared ternary FeF3–MgF2 materials have become promising heterogeneous catalysts due to their porosity and surface Lewis/Brønsted acidity (bi-acidity). Despite the good catalytic performance, nanoscopic characterisations of this type of material are still missing and the key factors controlling the surface properties have not yet been identified, impeding both a better understanding and further development of ternary fluoride catalysts. In this study, we characterised the interaction between the bi-acidic component (FeF3) and the matrix (MgF2) on the nano-scale. For the first time, the formation pathway of FeF3–MgF2 was profiled and the template effect of MgF2 during the synthesis process was discovered. Based on these new insights two novel materials, FeF3–CaF2 and FeF3–SrF2, were established, revealing that with decreasing the atomic numbers (from Sr to Mg), the ternary fluorides exhibited increasing surface acidity and surface area but decreasing pore size. These systematic changes gave rise to a panel of catalysts with tuneable surface and bulk properties either by changing the matrix alkaline earth metal fluoride or by adjusting their ratios to Fe or both. The template effect of the alkaline earth metal fluoride matrix was identified as the most probable key factor determining the surface properties and further influencing the catalytic performance in ternary fluoride based catalysts, and paves the way to targeted design of next-generation catalysts with tunable properties.
Die Synthetic Aperture Focusing Technique (SAFT) ist ein Verfahren zur Verarbeitung von HF-Bildern, die an unterschiedlichen Prüfkopfpositionen aufgenommen wurden. Es wird in der zerstörungsfreien Werkstoffprüfung genutzt, um eine Abbildung von Materialfehlern innerhalb des Gebietes zu erstellen, auf das die Rekonstruktion angewandt wird. Die nach Abschluss der SAFT-Rekonstruktion zusammengestellten Informationen über Reflektoren liegen zunächst nach wie vor in Form von HF-Daten vor. Die Interpretierbarkeit der SAFT-Bilder ist im Allgemeinen davon abhängig, wie diese Daten vor der endgültigen Darstellung aufbereitet werden. Die Bildung der Amplitudeneinhüllenden aus dem zugehörigen analytischen Signal stellt eine Möglichkeit einer solchen Aufbereitung nach Anwendung des SAFT-Algorithmus dar. Sie ist jedoch nur im eindimensionalen Fall eindeutig definiert. In diesem Beitrag wird das Konzept der analytischen Signale mit single-orthant-Spektren aufgegriffen, um eine Detektion der Einhüllenden an mehrdimensionalen HF-Daten durchzuführen. Dabei wird über die Betragsquadrate aller möglichen nach dieser Definition zu bildenden analytischen Signale gemittelt. Es wird gezeigt, dass die Anwendung des beschriebenen Verfahrens einem Separationsansatz entspricht. Außerdem wird eine Möglichkeit aufgezeigt die Gültigkeit dieses Ansatzes anhand der totalen und partiellen Hilberttransformationen des Signals im konkreten Fall zu überprüfen. Die Ergebnisse dieser Methode zur Verbesserung von SAFT Bildern werden unter Verwendung synthetischer und experimenteller Daten an rekonstruierten Abbildungen verschiedener Reflektorarten beispielhaft dargestellt.
Measurement of spontaneous magnetic stray field signals has been reported to be a promising tool for capturing macro-scale information of deformation states, defects and stress concentration zones in a material structure. This paper offers a new method for self-magnetic leakage field detection using a magneto-optical (MO) hand-held microscope. Its sensor has a dynamic field range between ±0.05 and ±2 kA/m and a lateral optical resolution of approx. 10 µm. We examined flat tensile test specimens of metastable austenitic steel AISI 304. Static tensile tests were repeatedly interrupted at various predetermined states of strain and the magnetic information was measured by the MO system. Comparative measurements using a high-precision magnetic field GMR-sensor, verify the outstanding capability of the MO microscope regarding spatial resolution of magnetic fields.
The Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), a Directorate General of the European Commission, operates the International Measurement Evaluation Program (IMEP). IMEP organises inter-laboratory comparisons in support of European Union policies. This paper presents the results of two proficiency tests (PTs): IMEP-116 and IMEP-39, organised for the determination of total Cd, Pb, As, Hg and inorganic As (iAs) in mushrooms. Participation in IMEP-116 was restricted to National Reference Laboratories (NRLs) officially appointed by national authorities in European Union member states. IMEP-39 was open to all other laboratories wishing to participate. Thirty-seven participants from 25 countries reported results in IMEP-116, and 62 laboratories from 36 countries reported for the IMEP-39 study. Both PTs were organised in support to Regulation (EC) No. 1881/2006, which sets the maximum levels for certain contaminants in food. The test item used in both PTs was a blend of mushrooms of the variety shiitake (Lentinula edodes). Five laboratories, with demonstrated measurement capability in the field, provided results to establish the assigned values (Xref). The standard uncertainties associated to the assigned values (uref) were calculated by combining the uncertainty of the characterisation (uchar) with a contribution for homogeneity (ubb) and for stability (ust), whilst uchar was calculated following ISO 13528. Laboratory results were rated with z- and zeta (ζ)-scores in accordance with ISO 13528. The standard deviation for proficiency assessment, σp, ranged from 10% to 20% depending on the analyte. The percentage of satisfactory z-scores ranged from 81% (iAs) to 97% (total Cd) in IMEP-116 and from 64% (iAs) to 84% (total Hg) in IMEP-39.
In- and quasielastic neutron scattering is employed to investigate both the vibrational density of states and the molecular dynamics of two homologous discotic liquid crystals (DLC) with different length of the alkyl side chain based on a triphenylene derivate. For both compounds characteristic low frequency excess contributions to the vibrational density of states are found. Therefore it is concluded that these liquid crystals show a glass-like behaviour. Elastic scans further show that in these materials a rich molecular dynamics takes place.
Polyglycerol (PG) coated polypropylene (PP) films were synthesized in a two-step approach that involved plasma bromination and subsequently grafting hyperbranched polyglycerols with very few amino functionalities. The influence of different molecular weights and density of reactive linkers were investigated for the grafted PGs. Longer bromination times and higher amounts of linkers on the surface afforded long-term stability. The protein adsorption and bacteria attachment of the PP-PG films were studied. Their extremely low amine content proved to be beneficial for preventing bacteria attachment.
In order to assess the anisotropy-related uncertainties of relatively determined photoluminescence quantum yields (ΦPL) of molecular emitters and luminescent nanomaterials, we compared ΦPL values measured without and with polarizers using magic angle conditions and studied systematically the dependence of the detected emission intensity on the polarizer settings for samples of varying anisotropy. This includes a dispersion of a spherical quantum dot (QD) with an ideally isotropic emission, a solution of a common small organic dye in a fluid solvent as well as dispersions of elongated quantum dot rods (QDR) with an anisotropic luminescence and a small organic dye in a rigid polymeric matrix, as ideally anisotropic emitter. Our results show that for instruments lacking polarizers, anisotropy-related measurement uncertainties of relative photoluminescence quantum yields can amount to more than 40%, with the size of these systematic errors depending on the difference in emission anisotropy between the sample and the standard.
Ergopeptides, like ergocornine and a-ergocryptine, exist in an S- and in an R-configuration. Kinetic experiments imply that certain configurations are preferred depending on the solvent. The experimental methods are explained in this article. Furthermore, computational methods are used to understand this configurational preference. Standard quantum chemical methods can predict the favored configurations by using minimum energy calculations on the potential energy landscape. However, the explicit role of the solvent is not revealed by this type of methods. In order to better understand its influence, classical mechanical molecular simulations are applied. It appears from our research that 'folding' the ergopeptide molecules into an intermediate state (between the S- and the R-configuration) is mechanically hindered for the preferred configurations.
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.
In this work an air-based sensor network for the localization of persons at extensive areas is presented. The developed network consists of a localization device which the person is wearing (BodyGuard-System), a mobile relay station in the air, and a base station. All three parts communicate with the same radio chip. The BodyGuard-System is an inertial navigation system which was developed for localization in difficult environments with high accuracy and low measurement uncertainty. To increase the range of the system, a multi-hop network was built up. The measured data of the BodyGuard-System and the mobile relay station is visualized on a PC in the base station. This multi-hop network is necessary for example for fire department missions.
The adsorption of porphyrin derivatives on a Au(111) surface was studied by scanning tunneling microscopy and spectroscopy at low temperatures in combination with density functional theory calculations. Different molecular appearances were found and could be assigned to the presence of single gold adatoms bonded by a coordination bond underneath the molecular monolayer, causing a characteristic change of the electronic structure of the molecules. Moreover, this interpretation could be confirmed by manipulation experiments of individual molecules on and off a single gold atom. This study provides a detailed understanding of the role of metal adatoms in surface–molecule bonding and anchoring and of the appearance of single molecules, and it should prove relevant for the imaging of related molecule–metal systems.
Bei der Abschätzung der Beständigkeit von Kunststoffen gegenüber niedermolekularen Flüssigkeiten ist die Kohäsionsenergiedichte CED ein wichtiger Parameter auf molekularer Ebene. Die Vernetzungsdichte ν eines polymeren Festkörpers bildet hierbei einen bedeutsamen Kennwert, der darüber hinaus neben der Löslichkeit wichtige Eigenschaften wie thermische Stabilität und Steifigkeit des Materials charakterisiert. Für die experimentelle Bestimmung von CED und ν eignet sich die Untersuchung des Quellverhaltens in unterschiedlichen Lösungsmitteln. Es werden zwei Messmethoden miteinander verglichen und die Ergebnisse unter Berücksichtigung des molekularen Aufbaus von Proben aus Polyurethan (PU) und hochmolekularem – (HMWPE) und ultrahochmolekularem Polyethylen (UHMWPE) diskutiert. Zum Verständnis des Quellverhaltens dieser Polymerproben in niedermolekularen Lösungsmitteln werden neben den Messergebnissen Literaturdaten zu Grunde gelegt.
We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand.
Quantitative determination of acidic surface sites is highly important for the characterization of solid acids because the activity of a catalyst is often related to the concentration of these sites. A recently developed method using 15N Nuclear Magnetic Resonance spectroscopy (NMR) for the quantification of acidic Lewis and Brønsted sites has been tested for a series of nanoscopic aluminum hydroxide fluorides. Comparison with other methods for the quantitative determination of acidic sites shows that this 15N NMR quantification method is a promising technique for the comprehensive investigation of acidic sites. Three different acidic sites, one Brønsted and two Lewis sites, can be distinguished by their 15N chemical shifts of pyridine and simultaneously quantified under conditions corresponding to catalytic reaction conditions. Determination of the individual concentrations of acidic sites allows further insight into the catalytic process. It was found that the concentration of Brønsted sites correlates with catalyzed conversion of citronellal to isopulegol in the investigated series of catalysts. Additionally, investigations indicate that one of the Lewis sites become blocked during the reaction of citronellal.
The digital photography has almost completely substituted the film photography. The film replacement is also fast progressing in medical X-ray radiography. This process is slower in NDT and especially in Europe. Reasons for the hesitating change to digital radiography (RT-D) in NDT are the necessary time for adoption of standards and the conservative request for film RT by auditors and NDT managers for applications in large plants and at construction areas. The fast serial inspection for small castings is already almost completely dominated by RT-D due to the cost effective short exposure and interpretation times. Standards were developed in parallel at CEN, ISO, ASTM and ASME. Unfortunately, the standard practices are different and the requirements on image quality and useable hardware are different too. The first standard series on Computed Radiography were developed and published by CEN and ASTM in 2005. Harmonized classification and qualification standards are available but the published practices are different. ASTM has developed the first standards for application of Digital Detector Arrays (DDA) in 2010. The first digital RT ISO standard practice is ISO 17636-2 (2013), which describes the practice for application of DDAs and Imaging Plates for weld inspection. At the first time this standard provides requirements for the selection of suitable hardware. Minimum image quality requirements are specified in analogy to film radiography and 3 Compensation Principles are defined to enable the application of a wider range of digital detectors. A comparison of the different international digital RT standards is given and first experiences with ISO 17636-2 are discussed. New standards on RT wall thickness and corrosion measurements (EN 16407, film and digital) have been developed recently.
A comparative study on the performance of digital detector systems for high energy applications
(2014)
For cast components reaching or exceeding total material thicknesses of 150mm, high energy sources such as linear accelerators or Betatrons are required in order to obtain reasonable exposure times. In this study, the performance of digital detector systems, involving imaging plates (IP) and digital detector arrays (DDA), was evaluated with respect to the testing class B requirements as formulated in the standard EN ISO 17636-2. As a reference, traditional radiographic film and a Cobalt-60 source was used. With film exposures, testing class B was achieved with Co-60 and Betatron (7.5 MV) at longer exposure times. The preliminary results show that the testing class B was not obtained with the examined digital detector arrays (DDA) and the high resolution imaging plates (IP) , even at 40, 60 and 80 minutes exposure time with a 7.5 MV Betatron. Class A was achieved using high resolution imaging plates with optimized metal filters between object and IPs and a high resolution DDA with intermediate Cu filters. Class A was also achieved applying a DDA with lower basic spatial resolution than required by Table B.13 of EN ISO 17636-2, but using the compensation principle as described in this standard. The next generation of digital detector arrays might potentially be able to obtain class B performance with the expected spatial resolution and sensitivity improvements.
The progress in X-ray detector electronics (sensitivity and speed) allows meanwhile fast single photon detection by a matrix detector. Combined photon counting and energy discrimination is implemented in the electronic circuit of each detector pixel. The company XCounter developed detectors based on CdTe single crystals, which can be tiled to larger areas and have a pixel size of 100ìm. The largest area available in beginning of 2014 is 50x75 mm². These detectors have very promising properties, which make them very suitable for NDT applications:
1. A CdTe attenuation layer of 750 µm thickness allows efficient X-ray detection up to ca. 300 keV. In counting mode only photon noise is important; no other detector noise sources need to be considered. There is no Offset signal without radiation.
2. Each of the detector pixels has two energy thresholds. These can be used for dual energy imaging for materials separation. Also the suppression of scattered radiation by energy thresholding will improve the image contrast sensitivity. First experiments will be presented which demonstrate the advantages of this new detector technology over the conventional charge integrating detectors.
A challenge is the development of a modified detector calibration procedure, which becomes critical at longer exposure times.
The objects of this investigation were sculptures taken from a ca. three hundred years old baroque epitaph of a church in Tonning, a town in Northern Germany. Around 1900 it was found in a disastrous state heavily damaged by wood-worm. At that time, the whole artwork was treated with the tar extract carbolineum as a remedy. Nowadays, this substance has been identified as carcinogenic, and its presence can be perceived by its stench and visually at certain spots on the surface where it has penetrated the covering paint.
A gold-painted sculpture of a massive wooden skull was interrogated with X-rays and fast neutrons to investigate the internal distribution of the carbolineum. The X-ray tomography, with its excellent spatial resolution revealed galleries left over from the worm infestation in the outer areas and cracks in the central region. The golden color coating appeared as a thick and dense layer. In comparison the tomography with fast neutrons, though being of lower resolution and yet unresolved artefacts revealed sections of slightly different densities in the bulk of the wood. These differences we attribute to the differences in the distribution of the impregnant in the wood, visible due to its higher hydrogen content making it less transparent for neutrons.
Using ultrafast X-ray diffraction, we study the coherent picosecond lattice dynamics of photoexcited thin films in the two limiting cases, where the photoinduced stress profile decays on a length scale larger and smaller than the film thickness. We solve a unifying analytical model of the strain propagation for acoustic impedance-matched opaque films on a semi-infinite transparent substrate, showing that the lattice dynamics essentially depend on two parameters: One for the spatial profile and one for the amplitude of the strain. We illustrate the results by comparison with high-quality ultrafast X-ray diffraction data of SrRuO3 films on SrTiO3 substrates.
Innovative X-ray backscatter technique for security applications: Detection of dangerous materials
(2014)
Radiological inspections, in general, are NDT&E methods to detect the bulk of explosives without invasion into the object of analysis. In contrast to personal luggage, cargo or structural components constitute a complexity that may significantly hamper the detection of a threat by conventional transmission radiography. A novel approach of interrogating a large object to a certain depth only with a single sided access will be presented. It consists of an X-ray backscatter camera with a special twisted slit collimator for imaging backscattered objects. The new X-ray backscatter camera is not only imaging the objects due to their densities but also by taking into account the influences of surrounding objects. Additionally, it does not only image illuminated features but also depicts shadows from absorbing materials. This is a unique characteristic of the developed X-ray backscatter camera. Experimental mock-ups are conducted imitating container with threats among a complex packing as they may be encountered in reality. At the end, the significant advantages of the presented X-ray backscatter camera in the context of aviation and port security will be discussed.
In this contribution, we present a dual high-energy X-ray imaging technique for cargo container inspection using the 'spectral high-energy X-ray attenuation method'. This method is based on attenuation of continuous highenergy spectra. The developed experimental technique consists of a betatron as high-energy (up to 7.5 MeV) X-ray source and a matrix detector with high spatial resolution (400 ìm) for digital X-ray imaging. In order to evaluate the material discrimination capability using dual high-energy X-ray imaging, a test specimen is proposed, comprising step wedges of different low and high atomic number (Z) materials. The selected X-ray spectra for the dual-energy experiments correspond to 3 MV and 7.5 MV acceleration potential of the betatron. We evaluated the ratio between low- and high-energy X-ray attenuation coefficients quantitatively based on simulated poly-energetic high-energy X-ray source spectra and the detector sensitivity using the 'analytical Radiographic Testing inspection simulation tool' (aRTist) developed at BAM. The simulated effective attenuation coefficients are compared with corresponding experimental results in order to establish a method for identification of low- and high-Z materials in the container. Finally, important applications of the proposed technique in the context of aviation security are discussed.
Critical parts in aircraft manufacturing such as stringers are very commonly used in modern aircraft structures to resist the compressive loads caused by the aerodynamic effects. They are generally made-up of thin aluminium (Al) metal sheets and are one of the key components in the aircraft wings. Any defects in the stringer leads to weakening of the stiffness of the whole wing structure and consequently, failures may occur. Hence, the structural integrity of the stringers should be evaluated using reliable non-destructive testing (NDT) methods. Due to the complex shaped structure of the stringer, the one-sided access NDT method such as X-ray backscatter technique is more preferable for the non-destructive imaging. In this paper, we present a new X-ray backscatter technique to image the internal sections of the stringer with only a single-sided access. The whole object was inspected by changing the viewing direction of the X-ray backscatter camera. For the first time, the X-ray backscatter measurements were conducted using high-energy (> 0.5MeV) X-rays and proved the applicability of the present technique to inspect thick carbon-fiber laminated components. In order to improve the inspection time and image quality of the backscatter image, we used high-resolution (180ìm) digital detector arrays (DDAs). At the end, important applications of the presented X-ray backscatter technique to the aerospace industry are discussed.
Genetic transformation of Knufia petricola A95 - a model organism for biofilm-material interactions
(2014)
We established a protoplast-based system to transfer DNA to Knufia petricola strain A95, a melanised rock-inhabiting microcolonial fungus that is also a component of a model sub-aerial biofilm (SAB) system. To test whether the desiccation resistant, highly melanised cell walls would hinder protoplast formation, we treated a melanin-minus mutant of A95 as well as the type-strain with a variety of cell-degrading enzymes. Of the different enzymes tested, lysing enzymes from Trichoderma harzianum were most effective in producing protoplasts. This mixture was equally effective on the melanin-minus mutant and the type-strain. Protoplasts produced using lysing enzymes were mixed with polyethyleneglycol (PEG) and plasmid pCB1004 which contains the hygromycin B (HmB) phosphotransferase (hph) gene under the control of the Aspergillus nidulans trpC. Integration and expression of hph into the A95 genome conferred hygromycin resistance upon the transformants. Two weeks after plating out on selective agar containing HmB, the protoplasts developed cell-walls and formed colonies. Transformation frequencies were in the range 36 to 87 transformants per 10 µg of vector DNA and 106 protoplasts. Stability of transformation was confirmed by sub-culturing the putative transformants on selective agar containing HmB as well as by PCR-detection of the hph gene in the colonies. The hph gene was stably integrated as shown by five subsequent passages with and without selection pressure.
Thermally reduced graphite oxide (TRGO), containing only four single carbon layers on average, was combined with ammonium polyphosphate (APP) and magnesium hydroxide (MH), respectively, in polypropylene (PP). The nanoparticle's influence on different flame-retarding systems and possible synergisms in pyrolysis, reaction to small flame, fire behavior and mechanical properties were determined. TRGO has a positive effect on the yield stress, which is decreased by both flame-retardants and acts as a synergist with regard to Young's modulus. The applicability and effects of TRGO as an adjuvant in combination with conventional flame-retardants depends strongly on the particular flame-retardancy mechanism. In the intumescent system, even small concentrations of TRGO change the viscosity of the pyrolysing melt crucially. In case of oxygen index (OI) and UL 94 test, the addition of increasing amounts of TRGO to PP/APP had a negative impact on the oxygen index and the UL 94 classification. Nevertheless, systems with only low amounts (≤1 wt%) of TRGO achieved V-0 classification in the UL 94 test and high oxygen indices (>31 vol%). TRGO strengthens the residue structure of MH and therefore functions as a strong synergist in terms of OI and UL 94 classification (from HB to V-0).
In this article, the high potential of the fluorolytic sol–gel process to synthesize nanoscopic rare earth-doped calcium fluoride sols is shown. Through a fluorolytic sol–gel process we manage to achieve spherical monodisperse ~5 nm sized nanoparticles using a simple and reproducible one-pot-wet chemical route at room temperature. The as-synthesized clear sols exhibit an intense red and green luminescence under UV excitation at room temperature. A spectroscopic study of the sols revealed the characteristic transitions 5D0 → 7FJ of Eu3+ and 5D4 → 7FJ of Tb3+, with 5D0 → 7F2 (611 nm) of Eu3+ and 5D4 → 7F4 (581 nm) of Tb3+ as the most prominent transitions. This facile synthetic strategy is also valuable for developing other luminescent nanoparticles.
Der Large Hadron Collider (LHC) des europäischen Kernforschungszentrums CERN ist einer der weltweit größten und leistungsfähigsten Teilchenbeschleuniger. Um den Teilchenstrahl auf seiner Kreisbahn zu halten, werden mit Hilfe supraleitender Spulen sehr starke Magnetfelder erzeugt. Die hierzu benötigten hohen Ströme werden über Verbunddrähte aus Niob-Titan und Kupfer geleitet.
Die Drähte werden u.a. durch Ultraschallschweißungen miteinander verbunden. Eine mangelhafte Verbindung kann zur Erwärmung der Kontaktstelle und in Folge davon zum Zusammenbruch der Supraleitung führen. Auf Anfrage des CERN wurden an der BAM Untersuchungen zur Prüfbarkeit solcher Verbindungen bei Umgebungstemperatur durchgeführt. Es gelang, für einen Verbindungstypen einen Wirbelstromsensor für eine manuelle Prüfung zu entwickeln. Ein Prototyp des Sensors befindet sich beim CERN in der praktischen Erprobung. Das Sensorprinzip sowie Prüfergebnisse aus Labor und Praxis werden vorgestellt.
A flexible, sustainable, one-step thermal decomposition route for the synthesis of hierarchical, heteroatom doped carbon foams is presented. Task-specific semi-organic crystals combine functions for three different purposes: the carbon and heteroatom source, a foaming agent (CO2) and an in situ generable template (NaCl). Insights to the decomposition pathway were gained through FTIR/MS coupled TGA and an ultrafast out-of-furnace heating procedure and the products were analysed with (HR)SEM/TEM, EELS, FTIR, and N2 sorption. The resulting macroporous carbon foams are excellent supports for metallic nanoparticles due to their hierarchical structure, high surface area and tuneable heteroatom contents. This was demonstrated for catalytically active copper or the magnetic CoNi alloy for water purification.
Structural properties of iron-phosphate glasses: spectroscopic studies and ab initio simulations
(2014)
Vitrification is the most effective method for the immobilization of hazardous waste by incorporating toxic elements into a glass structure. Iron phosphate glasses are presently being considered as matrices for the storage of radioactive waste, even of those which cannot be vitrified using conventional borosilicate waste glass. In this study, a structural model of 60P2O5–40Fe2O3 glass is proposed. The model is based on the crystal structure of FePO4 which is composed of [FeO4][PO4] tetrahedral rings. The rings are optimized using the DFT method and the obtained theoretical FTIR and Raman spectra are being compared with their experimental counterparts. Moreover, the proposed model is in very good agreement with X-ray absorption fine structure spectroscopy (XANES/EXAFS) and Mössbauer spectroscopy measurements. According to the calculations the Fe3+ is in tetrahedral and five-fold coordination. The maximal predicted load of waste constituents into the glass without rebuilding of the structure is 30 mol%. Below this content, waste constituents balance the charge of [FeO4]- tetrahedra which leads to their strong bonding to the glass resulting in an increase of the chemical durability, transformation and melting temperatures and density.
Rigid rod-type metallo-supramolecular coordination polyelectrolytes with Fe(II) centres (Fe-MEPEs) are produced via the self-assembly of the ditopic ligand 1,4-bis(2,2':6',2''-terpyridine-4'-yl)benzene (tpy-ph-tpy) and Fe(II) acetate. Fe-MEPEs exhibit remarkable electrochromic properties; they change colour from blue to transparent when an electric potential is applied. This electrochemical process is generally reversible. The blue colour in the ground state is a result of a metal-to-ligand charge transfer at the Fe(II) centre ion in a quasi-octahedral geometry. When annealed at temperatures above 100 °C, the blue colour turns into green and the formerly reversible electrochromic properties are lost, even after cooling down to room temperature. The thermally induced changes in the Fe(II) coordination sphere are investigated in situ during annealing of a solid Fe-MEPE using X-ray absorption fine structure (XAFS) spectroscopy. The study reveals that the thermally induced transition is not accompanied by a redox process at the Fe(II) centre. From the detailed analysis of the XAFS spectra, the changes are attributed to structural changes in the coordination sphere of the Fe(II) site. In the low temperature state, the Fe(II) ion rests in a quasi-octahedral coordination environment surrounded by six nitrogen atoms of the pyridine rings. The axial Fe–N bond length is 1.94 Å, while the equatorial bond length amounts to 1.98 Å. In the high temperature state, the FeN6-site exhibits a distortion with the axial Fe–N bonds being shortened to 1.88 Å and the equatorial Fe–N bonds being elongated to 2.01 Å.
-Background-
Laboratory leaching tests on treated wood were performed during a European robustness study in the framework of the validation of a tank leaching test procedure that has been proposed for construction products in order to determine the potential release of dangerous substances which can be transferred to soil and groundwater. The release of substances has to be determined also for materials treated with biocidal products according to the requirements of the European Biocidal Products Regulation. A similar leaching test procedure was already harmonised for treated wood for this purpose. Both test procedures were applied in parallel to wood treated with the same preservative to investigate whether the results of these tests can replace each other. Additional experiments were performed to further investigate unexpected effects of L/A ratio on leaching of copper and duration of storage of treated test specimens.
-Results-
Both procedures generate similar results concerning cumulative emissions of tebuconazole, copper, dissolved organic carbon and total nitrogen. The emission rates with time are in comparable ranges for both leaching protocols. Emissions of copper increased with decreasing L/A ratios. Strong correlation of copper concentrations and dissolved organic carbon as well as total nitrogen concentrations in eluates indicates that this observation is caused by co-elution of copper with organic substances. Duration of storage of treated test specimens affected emissions for the investigated wood preservative.
-Conclusions-
Based on these findings, results from both test procedures can be used to describe leaching characteristics and avoid double testing of treated wood to fulfil the requirements of the European regulations for either biocides or construction products. Leaching of substances from treated wood is a complex process that depends on its chemical composition and ageing processes.
Ultrasonic testing of adhesively bonded joints using air-coupled cellular polypropylene transducers
(2014)
In air-coupled ultrasonic testing, the impedance mismatch between the transducer and the air is commonly being solved by adding matching layers to composite transducers. To avoid the difficult technological procedure regarding matching layers, some new piezoelectric materials have been proposed. Most promising are ferroelectrets, which are charged cellular polymers, having ferroelectric and consequently piezoelectric properties. In particular, the extreme softness of cellular polypropylene (cPP) leads to a high piezoelectric constant and to a good impedance match with the air, making matching layers redundant. Its elasticity modulus below 1 MPa causes an additional effect not observed with common piezoelectric materials: that is the electrostrictive effect, here defined as the thickness change due to the attractive force between the transducer electrodes. This effect exceeds the piezoelectric effect at excitation voltages over 1 kV. The extreme softness of cPP leads also to high flexibility, enabling easy focusing by bending the transducer.
We have developed air-coupled ultrasonic transducers based on cPP. This includes the electrical matching networks for the transmitter and for the receiver. The transmitter is excited with voltages up to 2.5 kV, so that the electrostrictive effect dominates, leading to sound pressure around 145dB at the transducer surface. These transducers have been applied for testing carbon-fiber-reinforced polymer plates, adhesive joints and other composite structures. Here we report about ultrasonic transmission of two types of adhesive joints. The first one is multi-layer aluminium components with some artificial disbonds, which are common in aerospace industry, and the second one is an aluminium-steel joint with polyurethane adhesive, which is used in automotive industry.
Pore annihilation was investigated in the single-crystal nickel-base superalloy CMSX-4. HIP tests at 1288 °C/103 MPa were interrupted at different times, then the specimens were investigated by TEM, metallography and density measurements. The kinetics of pore annihilation was determined. The pore closure mechanism was identified as plastic deformation on the octahedral slip systems. A model describing the kinetics of pore closure has been developed on the base of crystal plasticity and large strain theory. Mechanical tests with the superalloy CMSX-4 and the Ru-containing superalloy VGM4 showed, that HIP significantly increases the fatigue life at low temperatures but has no effect on creep strength.
The combination of complementary characterization techniques such as SEM (Scanning Electron Microscopy), T-SEM (Scanning Electron Microscopy in Transmission Mode), EDX (Energy Dispersive X-ray Spectroscopy) and SAM (Scanning Auger Microscopy) has been proven to be a powerful and relatively quick characterization strategy for comprehensive morphological and chemical characterization of individual silica and titania nanoparticles. The selected real life test materials, silica and titania, are listed in the OECD guidance manual as representative examples because they are often used as commercial nanomaterials. Imaging by high resolution SEM and in the transmission mode by T-SEM allows almost simultaneous surface and in-depth inspection of the same particle using the same instrument. EDX and SAM enable the chemical characterization of bulk and surface of individual nanoparticles. The core–shell properties of silica based materials are addressed as well. Titania nominally coated by silane purchased from an industrial source has been found to be inhomogeneous in terms of chemical composition.
The tribological and mechanical properties of niobium carbides (NbC) bonded with cobalt of Fe3Al
(2014)
The tribological and mechanical properties of niobium carbide bonded with 8 vol.-% (NbC-8Co), 12 vol.-% of cobalt (NbC-12Co) or 12 vol.-% of Fe3Al (NbC-12Fe3Al) are presented. Rotating discs made of metal-bonded niobium carbide were mated against alumina (99.7%) under unlubricated (dry) unidirectional sliding tests (0.1 m/s to 12.0 m/s; 22 °C and 400 C) as well as in oscillation tests (f=20 Hz, Δx=0.2 mm, 2/50/98% rel. humidity, n=105/106 cycles). Microstructure and phase compositions were determined as well. The tribological data obtained were benchmarked with different ceramics, cermets, hard metals and thermally sprayed coatings, where NbC bonded with 8% and 12% Co presented above 7 m/s the lowest wear rates so far in such a benchmark. Binderless NbC (HP-NbC1) and the metal-bonded NbCs exhibited low wear rates under dry sliding associated with P·V high load carrying capacities. NbC-based hard metal bonded with 12 vol.-% of Fe3Al resulted in a higher hardness level than for 12 vol.-% cobalt. The tribological profile established revealed a strong position of NbC-bearing materials under tribological considerations and for closed tribosystems against established reference tribo-couples.
Two design approaches for multifunctional information carriers are introduced. In the first one, quick response (QR) code carriers, which were composed of poly(ester urethane) (PEU) and microencapsulated thermochromic pigments (T-PIGs), differing in color and color switching temperature (CST), were prepared. The obtained material systems exhibited machine-readable QR codes at 23 °C and a two-stage decolorization when heated, culminating in unreadable QR codes at temperatures above the highest CST of the employed T-PIGs. In the second scenario, information carriers were sealed with a dark, thermochromic PEU layer. As a result, the QR codes were hidden at 23 °C and became readable upon heating due to color fading. Beyond the characterization of the employed components, preparation methods, functionality analyses and durability investigations are reported. When heated after thermo-mechanical programming, pronounced shape memory properties could be verified. The thermo-responsiveness of such multifunctional material systems may qualify them for usage in anti-counterfeiting applications.
The objective of this study was to investigate the influence of externally applied magnetic fields on the weld quality in laser beam welding. The optimization of the process parameters was performed using the results of computer simulations. Welding tests were performed with up to 20 kW laser beam power. It was shown that the AC magnet with 3 kW power supply allows for a prevention of the gravity drop-out for full penetration welding of 20 mm thick stainless steel plates. For partial penetration welding it was shown that an0.5 T DC magnetic field is enough for a suppression of convective flows in the weld pool. Partial penetration welding tests with 4 kW beam power showed that the application of AC magnetic fields can reduce weld porosity by a factor of 10 compared to the reference joints. The weld surface roughness was improved by 50%.
DNA origami nanostructures allow for the arrangement of different functionalities such as proteins, specific DNA structures, nanoparticles, and various chemical modifications with unprecedented precision. The arranged functional entities can be visualized by atomic force microscopy (AFM) which enables the study of molecular processes at a single-molecular level. Examples comprise the investigation of chemical reactions, electron-induced bond breaking, enzymatic binding and cleavage events, and conformational transitions in DNA. In this paper, we provide an overview of the advances achieved in the field of single-molecule investigations by applying atomic force microscopy to functionalized DNA origami substrates.
The most successful additive manufacturing (AM) technologies are based on the layer-by-layer deposition of a flowable powder. Although considered as the third industrial revolution, one factor still limiting these processes to become completely autonomous is the often necessary build-up of support structures. Besides the prevention of lateral shifts of the part during the deposition of layers, the support assures quality and stability to the built process. The loose powder itself surrounding the built object, or so-called powder-bed, does not provide this sustenance in most existent technology available. Here we present a simple but effective and economical method for stabilizing the powder-bed, preventing distortions in the geometry with no need for support structures. This effect, achieved by applying an air flow through the powder-bed, is enabling an entirely autonomous generation of parts and is a major contribution to all powder-based additive manufacturing technologies. Moreover, it makes powder-based AM independent of gravitational forces, which will facilitate crafting items in space from a variety of powdery materials.
Geführte Ultraschallwellen bieten eine Vielzahl von Einsatzmöglichkeiten in der Zerstörungsfreien Prüfung, der Zustandsüberwachung sowie der Materialcharakterisierung. Insbesondere für Rohrleitungen und ausgedehnte Plattenstrukturen ist eine Vielzahl von auf geführten Wellen basierenden Verfahren in der Entwicklung und teilweise bereits im Einsatz. Aufgrund des komplexen Ausbreitungsverhaltens geführter Wellen werden numerische Verfahren (etwa die Finite Elemente Methode (FEM) oder die Randelementemethode (BEM)) zur Simulation der Wellenausbreitung sowie der Wechselwirkung mit Defekten in Wellenleitern angewendet. Diese Methoden sind für große Strukturen extrem rechenintensiv und umständlich in der Anwendung. Ein ungleich effizienteres Verfahren wurde kürzlich von den Autoren auf Grundlage der Scaled Boundary Finite Element Method entwickelt. Ein semi-analytischer Ansatz erlaubt die Modellierung beliebig ausgedehnter Strukturen bei extrem kurzen Rechenzeiten. Die Wechselwirkung geführter Wellen mit Rissen kann auf besonders elegante und exakte Weise beschrieben werden. Mit dieser Methode können die komplexen Vorgänge in Wellenleitern innerhalb weniger Sekunden modelliert werden.
Fourier-Spektroskopische Untersuchungen von hochmolekularem Polyethylen (HMW-PE) und ultrahochmolekularem Polyethylen (UHMW-PE) im Mittleren - und Fernen Infrarotbereich können Veränderungen der molekularen Strukturen nachweisen, die durch Co60 γ-Strahlung und Rekristallisationsprozesse initiiert werden. UHMW-PE und HMW-PE sind im gewählten IR-Bereich unterscheidbar. Die integrale Absorption der B1u – Gitterschwingungen im Fernen Infrarotbereich (THz-Bereich) ermöglichen die quantitative Beschreibung des Kristallinitätsgrades und dessen Abbau. Die Bildung ungesättigter Vinylengruppen und der Abbau ungesättigter Methylengruppen können im Mittleren Infrarotbereich nachgewiesen werden.
The synthesis of the polymorphic cocrystal caffeine:anthranilic acid was investigated to obtain a better understanding of the processes leading to the formation of different polymorphic forms. In the case of these cocrystal polymorphs synthesized by liquid-assisted grinding a distinct influence of the dipole moment of the solvent was found. A pre-coordination between the solvent molecules and the caffeine:anthranilic acid cocrystal could be identified in the formation of form II. In the case of form II the solvent can be regarded as a catalyst. The formation pathway of each polymorph was evaluated using synchrotron X-ray diffraction.
Bikontinuierliche poröse Keramiken für Filteranwendungen weisen eine komplizierte Mikrostruktur auf, in der Poren und Festkörperphase 'vermischt' sind. Mechanische, thermische sowie Filtereigenschaften können nur präzise bestimmt werden, wenn die Morphologie beider Phasen quantitativ angegeben werden kann. Hier werden unter Anwendung von 3D Computertomographie (CT) und verschiedenen Techniken, die auf der Röntgenrefraktion basieren, die Porosität und die Porenorientierung in keramischen Cordierit-Dieselpartikelfiltern bewertet. Dabei werden zur Auswertung der Tomogramme die Fouriertransformierten sowie eine neu entwickelte richtungssensitive Bildanalyse (DIVA, directional interface variance analysis) angewandt. Sowohl die genannten Messtechniken als auch der statistische Ansatz gestatten die Extraktion optional ortsaufgelöster oder gemittelter Werte. Es ergeben sich sehr gute Übereinstimmungen der experimentell ermittelten Porositätswerte mit Ergebnissen aus Quecksilberintrusionsversuchen als auch der ermittelten Porenorientierung im Vergleich zu publizierten Angaben zur kristallographischen Textur. Dies legt den Schluss nahe, dass die Kenntnis der Grenzflächen (zwischen Poren und Materie) genügt, die morphologischen Eigenschaften solcher Materialien hinreichend zu beschreiben.
The determination of the fatigue life in technical alloys containing large and small defects must rely on a propagation model which accounts for short and long crack growth. Recently an analytical model which incorporates propagation in the short crack regime and plastic correction for the crack driving force has been presented by two of the authors.
This work is intended to show further validation of the model, taking into account data sets for different materials with different testing conditions.
Despite the assumptions about missing parameters, the value of which had to be taken from the literature, the predictions showed a fairly good approximation of the fatigue lives. A possible interpretation of the results in terms of multiple crack initiation and propagation at higher loads is proposed.
A micromechanical model of creep induced grain boundary damage is proposed, which allows for the simulation of creep damage in a polycrystal with the finite element method. Grain boundary cavitation and sliding are considered via a micromechanically motivated cohesive zone model, while the grains creep following the slip system theory. The model has been calibrated with creep test data from pure Cu single crystals and a coarse-grained polycrystalline Cu-Sb alloy. The test data includes porosity measurements and estimates of grain boundary sliding. Finally, the model has been applied to Voronoi models of polycrystalline structures. In particular the influence of grain boundary sliding on the overall creep rate is demonstrated.
Recently, C K-edge Near Edge X-ray Absorption Fine Structure (NEXAFS) spectra of graphite (HOPG) surfaces have been measured for the pristine material, and for HOPG treated with either bromine or krypton plasmas (Lippitz et al., Surf. Sci., 2013, 611, L1). Changes of the NEXAFS spectra characteristic for physical (krypton) and/or chemical/physical modifications of the surface (bromine) upon plasma treatment were observed. Their molecular origin, however, remained elusive. In this work we study by density functional theory, the effects of selected point and line defects as well as chemical modifications on NEXAFS carbon K-edge spectra of single graphene layers. For Br-treated surfaces, also Br 3d X-ray Photoelectron Spectra (XPS) are simulated by a cluster approach, to identify possible chemical modifications. We observe that some of the defects related to plasma treatment lead to characteristic changes of NEXAFS spectra, similar to those in experiment. Theory provides possible microscopic origins for these changes.
Hemocompatible materials are needed for internal and extracorporeal biomedical applications, which should be realizable by reducing protein and thrombocyte adhesion to such materials. Polyethers have been demonstrated to be highly efficient in this respect on smooth surfaces. Here, we investigate the grafting of oligo- and polyglycerols to rough poly(ether imide) membranes as a polymer relevant to biomedical applications and show the reduction of protein and thrombocyte adhesion as well as thrombocyte activation. It could be demonstrated that, by performing surface grafting with oligo- and polyglycerols of relatively high polydispersity (>1.5) and several reactive groups for surface anchoring, full surface shielding can be reached, which leads to reduced protein adsorption of albumin and fibrinogen. In addition, adherent thrombocytes were not activated. This could be clearly shown by immunostaining adherent proteins and analyzing the thrombocyte covered area. The presented work provides an important strategy for the development of application relevant hemocompatible 3D structured materials.
Über die Entwicklung von Anwendungsregeln für reaktive Brandschutzsysteme auf Stahlzuggliedern
(2014)
Der vorliegende Beitrag stellt den Entwicklungsstand von Anwendungsregeln für reaktive Brandschutzsysteme auf Stahlzuggliedern zusammenfassend dar. Dabei wird insbesondere auf die jüngsten Veränderungen in den normativen Grundlagen und bauaufsichtlichen Regelungen eingegangen und im Hinblick auf Sicherheitsaspekte bewertet.
Die Verringerung der Teilsicherheit für den Bauteilwiderstand nicht stabilitätsgefährdeter Bauteile im Regelwerk für die Kaltbemessung von Stahltragwerken ist hier als besonders kritisch anzusehen, da hierdurch ein systematisches Sicherheitsdefizit für den Brandfall verursacht wird.
Weiterhin werden neuste Forschungsergebnisse bei der Entwicklung von Bewertungsregeln von reaktiven Brandschutzsystemen auf Vollkreisprofilen unter Zugbeanspruchung vorgestellt und diskutiert. Die Untersuchungen behandeln die Fragestellung, inwieweit Prüfungen mit Zugbeanspruchungen an Kreisvollprofilen erforderlich sein werden.
Sollten CT Aufnahmen quantitativ und automatisch ausgewertet werden, ist die Qualität der Tomogramme ein wesentlicher Punkt. Außerdem steht bei Serienmessungen nur eine begrenzte Meßzeit für jede Probe. Es werden die verschiedenen Mikrofokusröhren in Bezug auf die Parameter Orts- und Dichteauflösung, sowie Meßzeit verglichen, CT Beispiele dazu gezeigt.
In order to investigate molecular recognition on surfaces, an azide-functionalized monolayer was deposited on gold. The monolayer was characterized by X-ray photoelectron spectroscopy (XPS) and angle-resolved near-edge X-ray absorption fine structure (NEXAFS) experiments and the decomposition of the azide upon irradiation with X-ray beams was investigated. Subsequently, various alkyne-functionalized host and guest molecules were attached to the azide by 1,3-dipolar cycloaddition. These modified surfaces and their host–guest chemistry were analysed by XPS and angle-resolved NEXAFS. The reversibility of guest binding was shown for one example as a proof of principle.
The mechanochemical synthesis of two model compounds, a metal organic framework ([Bi(1,4-bdc)2]*(Im) (bdc = benzene dicarboxylate, Im = imidazole cation)) and a cocrystal (Carbamazepine:Indometacin 1:1) were followed ex situ by combined analytical methods. Powder X-ray diffraction (XRD) and Raman spectroscopy data were evaluated for the synthesis of the metal organic framework. XRD measurements and REM images were analysed for the synthesis of the cocrystal. The measurements revealed that both model compounds were synthesised within minutes. The metal organic framework [Bi(1,4-bdc)2]*(Im) is synthesised via an intermediate structure. The cocrystal Carbamazepine:Indometacin 1:1 is formed within few seconds and afterwards the crystallite size decreases extremely.
Two metal organic structures composed of the ligands benzene-1,4-dicarboxylate and pyridine-2,5-dicarboxylate and bismuth cations are presented: (H2Im)[Bi(1,4-bdc)2] (1) and [Bi(pydc)(NO3)2(H2O)2]*H2O (2) (bdc = benzenedicarboxylate, H2Im = imidazole cation, pydc = pyridinedicarboxylate). Both compounds were synthesised via grinding and the crystal structure of compound (2) was solved based on its powder diffraction pattern. Compound 1 crystallises isostructurally to the dimethyl ammonium containing compound (dma)[(Bi(1,4-bdc)2]. Raman spectroscopy and Extended X-ray absorption fine structure (EXAFS)
measurements provided additional information about the two mechanochemically synthesised metal organic compounds.
The current furfural production yield is low due to the use of non-selective homogeneous catalysts and expensive separation. In this work, partially hydroxylated MgF2 catalysts, synthesized using different water contents, were screened during xylose dehydration in watertoluene at 160 °C. The different Lewis/Brønsted ratios on the MgF2 catalysts showed that under-coordinated Mg can isomerize xylose to xylulose, whilst the surface OH-groups were responsible for the dehydration reactions. The presence of glucose as a co-carbohydrate reduced the furfural selectivity from 86 to 81%, whilst it also led to high 5-hydroxymethylfurfural selectivity. The tests catalyzed by MgF2 in combination with simultaneous N2-stripping showed that a furfural selectivity of 87% could be achieved using low xylose loadings. Moreover, the catalysts regenerated by H2O2 showed high activity during the dehydration tests in watertoluene at 160 °C.
Recent advances in vacuum sciences and applications are reviewed. Novel optical interferometer cavity devices enable pressure measurements with ppm accuracy. The innovative dynamic vacuum standard allows for pressure measurements with temporal resolution of 2 ms. Vacuum issues in the construction of huge ultra-high vacuum devices worldwide are reviewed. Recent advances in surface science and thin films include new phenomena observed in electron transport near solid surfaces as well as novel results on the properties of carbon nanomaterials. Precise techniques for surface and thin-film characterization have been applied in the conservation technology of cultural heritage objects and recent advances in the characterization of biointerfaces are presented. The combination of various vacuum and atmospheric-pressure techniques enables an insight into the complex phenomena of protein and other biomolecule conformations on solid surfaces. Studying these phenomena at solid–liquid interfaces is regarded as the main issue in the development of alternative techniques for drug delivery, tissue engineering and thus the development of innovative techniques for curing cancer and cardiovascular diseases. A review on recent advances in plasma medicine is presented as well as novel hypotheses on cell apoptosis upon treatment with gaseous plasma. Finally, recent advances in plasma nanoscience are illustrated with several examples and a roadmap for future activities is presented.
The vibrational density of states of a series of homologous triphenylene-based discotic liquid crystals HATn (n = 5, 6, 8, 10, 12) depending on the length of the aliphatic side chain is investigated by means of inelastic neutron scattering. All studied materials have a plastic crystalline phase at low temperatures, followed by a hexagonally ordered liquid crystalline phase at higher temperatures and a quasi isotropic phase at the highest temperatures. The X-ray scattering pattern for the plastic crystalline phase of all materials shows a sharp Bragg reflection corresponding to the intercolumnar distance in the lower q-range and a peak at circa 17 nm-1 related to intracolumnar distances between the cores perpendicular to the columns as well as a broad amorphous halo related to the disordered structure of the methylene groups in the side chains in the higher q-range. The intercolumnar distance increases linearly with increasing chain length for the hexagonal columnar ordered liquid crystalline phase. A similar behaviour is assumed for the plastic crystalline phase. Besides n = 8 all materials under study exhibit a Boson peak. With increasing chain length, the frequency of the Boson peak decreases and its intensity increases. This can be explained by a self-organized confinement model. The peaks for n = 10, 12 are much narrower than for n = 5, 6 which might imply the transformation from a rigid system to a softer one with increasing chain length. Moreover the results can also be discussed in the framework of a transition from an uncorrelated to a correlated disorder with increasing n where n = 8 might be speculatively considered as a transitional state.
This paper presents a finite element model of an overhead transmission line using so called cable elements which allow reproducing the cable's nonlinear characteristics accurately employing only a few elements. Aerodynamic damping is considered in the equation of motion by taking into account the relative velocity between the flow of the wind and the moving structure. The wind flow itself is simulated by wave superposition making necessary assumptions on the lateral correlation between the wind velocities along the cable length. As result from the simulation, the following conclusions can be drawn. The first natural frequency of generally used wide spanning cables lies well below 1 Hz where also most of the energy content of the wind excitation is to be expected. Aerodynamic damping is significant for the moving cables holding very low structural damping which leads to a suppression of resonant amplification. This is particularly of interest regarding the support reaction which is dominated by the mean value and the so called background response. The latter is mostly influenced by the randomness of the wind flow, especially lateral to the main wind direction.
A mechanical structure supported by nonlinear springs subjected to an external load is considered. If all mechanical parameters of the system were known, the displacement of the system subjected to this load could be easily calculated. If not all of the parameters are known, but the load and the displacement are measured at one location, an inverse problem exists. In the presented problem the nonlinear springs are unknown and have to be determined. At first glance a problem needs to be solved, which is underdetermined due to the number of unknown variables. However, evolutionary computing can be applied to solve this inverse, nonlinear and multimodal problem. Sometimes a prior knowledge exists on certain system properties, which is difficult to implement into analytical or numerical solver. This knowledge can play a decisive role in identifying the system properties and it can be easily included as boundary condition when applying evolutionary algorithm. This article examines how and under what conditions the spring resistances can be identified. The procedure is exemplified at a mechanical system of a pile foundation.
The observation of morphological details down to the nanometer range of the outer surface of micro-, submicro- and nanoparticles in a high-resolution scanning electron microscope (SEM) was extended with in-depth observation by enabling the transmission mode in the SEM, i.e. TSEM. The micro- and nanocapsules characterized in this study were fabricated as depots for protective agents to be embedded in innovative self-healing coatings. By combining the two imaging modes (upper and in-depth observation) complementing each other a better characterisation by a more comprehensive interpretation of the 'consistency' of the challenging specimens, e.g. including details 'hidden' beyond the surface or the real specimen shape at all, has been attained. Furthermore, the preparation of the quasi electron transparent samples onto thin supporting foils enables also elemental imaging by energy dispersive X-ray spectroscopy (EDX) with high spatial resolution. Valuable information on the elemental distribution in individual micro-, submicro- and even nanocapsules completes the '3D' high resolution morphological characterization at the same multimodal SEM/TSEM/EDX system.
In welding experiments conducted on heavy wall pipes, the penetration mode (full or partial penetration) occurred to be a significant factor influencing appearance of solidification cracks. To explain the observed phenomena and support further optimization of manufacturing processes, a computational model was developed, which used a sophisticated strategy to model the material. High stresses emerged in the models in regions which showed cracking during experiments. In partial penetration welding, they were caused by the prevention of weld shrinkage due to the cold and strong material below the joint. Another identified factor having an influence on high stress localization is bulging of the weld.
On the role of fluoro-substituted nucleosides in DNA radiosensitization for tumor radiation therapy
(2014)
Gemcitabine (2',2'-difluorocytidine) is a well-known radiosensitizer routinely applied in concomitant chemoradiotherapy. During irradiation of biological media with high-energy radiation secondary low-energy (<10 eV) electrons are produced that can directly induce chemical bond breakage in DNA by dissociative electron attachment (DEA). Here, we investigate and compare DEA to the three molecules 2'-deoxycytidine, 2'-deoxy-5-fluorocytidine, and gemcitabine. Fluorination at specific molecular sites, i.e., nucleobase or sugar moiety, is found to control electron attachment and subsequent dissociation pathways. The presence of two fluorine atoms at the sugar ring results in more efficient electron attachment to the sugar moiety and subsequent bond cleavage. For the formation of the dehydrogenated nucleobase anion, we obtain an enhancement factor of 2.8 upon fluorination of the sugar, whereas the enhancement factor is 5.5 when the nucleobase is fluorinated. The observed fragmentation reactions suggest enhanced DNA strand breakage induced by secondary electrons when gemcitabine is incorporated into DNA.
Das Monitoring von Bauteilen bei Ermüdungsbelastung mit Hilfe der Schallemission liefert eine große Anzahl an Schallemissionsdaten und –parametern. Um diese in einen Zusammenhang mit dem Schadenszustand des Bauteils zu bringen ist es sinnvoll, einen Bezug zu bekannten bruchmechanischen Kenngrößen herzustellen. Dies wird in dieser Arbeit anhand von Ermüdungsversuchen an Platten aus dem Feinkornstahl P460NL1 versucht. Schallemissionssignale aus Ermüdungsrissen mit und ohne Korrosionseinfluss werden analysiert und mit bekannten bruchmechanischen Kenngrößen wie der Risswachstumsrate und dem Spannungsintensitätsfaktor verglichen.
A method for the determination of very volatile organic compounds (VVOC) in air was developed and successfully tested for methanol and ethanol. Carbotrap300® (a multi-bed tube using Carbopack C®, Carbopack B® and Carbosive SIII®) was selected as sorption material for thermal desorption and tested for its suitability for emission test chamber measurements. The adsorption behaviour and the chromatographic results are influenced negatively by spiking aqueous solutions on the adsorption medium for calibration purposes. The latter effect can be reduced by blowing dry air across the adsorbent to remove the adsorbed water. Detection and quantification limits were determined for a GC-FID system and compared to GC-MS. The applicability of the method was tested with a methanol eliminating silane modified polymeric adhesive (SMP-adhesive for parquet) in an emission test chamber
Algal blooms are a frequent phenomenon in nearly all kinds of fresh water. Global warming and eutrophication by waste water, air pollution and fertilizers seem to lead to an increased frequency of occurrence. Many cyanobacteria produce hazardous and quite persistent toxins, which can contaminate the respective water bodies. This may limit the use of the raw water for many purposes. The purification of the contaminated water might be quite costly, which makes a continuous and large scale treatment economically unfeasible in many cases. Due to the obvious risks of algal toxins, an online or mobile detection method would be highly desirable. Several biosensor systems have been presented in the literature for this purpose. In this review, their mode of operation, performance and general suitability for the intended purpose will be described and critically discussed. Finally, an outlook on current developments and future prospects will be given.
Luminescence techniques are among the most widely used detection methods in the life and material sciences. At the core of these methods is an ever-increasing variety of fluorescent reporters (i.e., simple dyes, fluorescent labels, probes, sensors and switches) from different fluorophore classes ranging from small organic dyes and metal ion complexes, quantum dots and upconversion nanocrystals to differently sized fluorophore-doped or fluorophore-labeled polymeric particles. A key parameter for fluorophore comparison is the fluorescence quantum yield (Φf), which is the direct measure for the efficiency of the conversion of absorbed light into emitted light. In this protocol, we describe procedures for relative and absolute determinations of Φf values of fluorophores in transparent solution using optical methods, and we address typical sources of uncertainty and fluorophore class-specific challenges. For relative determinations of Φf, the sample is analyzed using a conventional fluorescence spectrometer. For absolute determinations of Φf, a calibrated stand-alone integrating sphere setup is used. To reduce standard-related uncertainties for relative measurements, we introduce a series of eight candidate quantum yield standards for the wavelength region of ~350950 nm, which we have assessed with commercial and custom-designed instrumentation. With these protocols and standards, uncertainties of 5–10% can be achieved within 2 h.
Für die optische Erwärmung von Prüfteiloberflächen sind Blitz- und Halogenlampen Stand der Technik. Der Vorteil dieser Wärmequellen liegt in ihren relativ geringen Anschaffungskosten bei gleichzeitig hohen Leistungsdichten am Prüfobjekt. Nachteilig ist bei den Halogenlampen die Limitierung der möglichen Modulationsffequenz auf ca. 1 Hz für die Anwendung dieser Quelle in der Lockin-Thermografie. Blitzlampen bieten für gewöhnlich nur eine feste Blitzdauer bei einer geringen Taktrate. Beide Anregungsquellen müssen in Reflexionsanordnung mit Filtern betrieben werden um die entstehende thermische Eigenstrahlung als Störquelle zu eliminieren. Wir stellen Untersuchungen an Hochleistungs-LEDs für den Einsatz in der aktiven Thermografie vor. Diese Lichtquellen werden durch die rasante Entwicklung der möglichen Leistungsdichten nun auch für die thermografische ZfP interessant. Sie zeigen ähnlich dem Laser eine schmale und auf den Werkstoff abstimmbare spektrale Verteilung der Strahlungsleistung bei moderaten Kosten. Die zugrunde liegende Elektrolumineszenz generiert kaum Wärmestrahlung und ermöglicht dadurch die Prüfung während des Erwärmungsvorganges ohne größeren Aufwand. Modulationsfrequenzen über 100 Hz mit thermischen Eindringtiefen < 1 mm sind möglich. Dadurch qualifizieren sich die LEDs zur Anwendung in der Lockin-Thermografie von Metallen und zur oberflächennahen Prüfung von Schichtsystemen. Durch die fast verzögerungsffeie Reaktion der LED auf das steuernde Signal sind nahezu beliebige zeitliche Anregungsformen möglich. Mit solch flexiblen Anregungsformen ließen sich bereits bei den photothermischen Verfahren erfolgreich höhere Tiefenreichweiten und -auflösungen gegenüber den klassischen Methoden der monofrequenten Lockin - und energiereichen Kurzimpuls-Anregung erzielen. Untersuchungen dieser Möglichkeiten im praktischen Einsatz der HochleistungsLEDs werden vorgestellt und mit herkömmlichen Lichtquellen verglichen.
Odour measurements become increasingly important in view of the assessment of indoor air quality and the emissions of building products. Hence they need to be implemented into evaluation schemes such as the AgBB scheme. While there are already standards like DIN ISO 16000-28 and VDI 4302 Part 1 specifying the procedure of odour measurements using a comparison scale, no final validation of the method has been carried out so far. Therefore, a round robin test was conducted in 2012 with 12 participating laboratories that mainly consisted of the following two parts: 1) testing of the available comparison scales with respect to their operational performance and 2) execution of an odour assessment of an acrylic sealant using emission test chambers. Part one included the measurement of the air flow rates and the provided concentrations of the reference substance (acetone). Part two was conducted to test the performance of the laboratories and the applicability of DIN ISO 16000-28 and supplementary VDI 4302 Part 1 by assessing the perceived intensity and the hedonic tone of the air samples. Moreover, samples for VOC analysis were taken from the air in the emission test chamber on the 7th day of testing to allow for quality control. Resulting from this round robin test main deficits were detected and suggestions for the improvement of the odour measurement procedure were made.
A major requirement for the validation of methods assessing the risk associated with engineered nanoparticles (ENPs) is the use of reference materials (RMs). In the present contribution we review available RMs, ongoing projects and characterisation trends in the field. The conclusion is that actual approaches to RMs mostly deal with metrological considerations about single properties of the ENPs, typically their primary size, which can hardly be representative of nanoparticles characteristics in real testing media and therefore, not valid for reliable and comparable toxicological studies. As an alternative, we discussed the convenience and feasibility of establishing multi-parametric RMs for a series of ENPs, focusing on silica nanoparticles (SNPs). As a future perspective, the need to develop RMs based on hybrid nanoparticles is also discussed.
PLR Prüftechnik Linke & Rühe Magdeburg und die BAM Bundesanstalt für Materialforschung und -prüfung Berlin haben in Zusammenarbeit mit anderen Partnern im Laufe der letzten Jahre verschiedene Wirbelstromsysteme zur Prüfung verlegter Schienen auf rissartige Fehler des Typs Head Checks entwickelt. Die Entwicklung dieser Systeme erfolgte mit dem Ziel, ein Hilfsmittel für die Planung von Schieneninstandhaltungsmaßnahmen zu schaffen. Die Systeme haben sich im praktischen Prüfeinsatz bewährt. Hierzu wurde regelmäßig auf den vorhergehenden Tagungen berichtet. Bei der Schieneninstandhaltung kommen unterschiedliche Typen von Schienenbearbeitungsmaschinen zum Einsatz, z. B. Schienenfräs- und Schleifzüge. Seit einiger Zeit wird von Seiten der Schienennetzbetreiber vermehrt ein Qualitätsnachweis nach erfolgter Schienenbearbeitung gefordert. Hierzu wurde ein Wirbelstromprüfsystem entwickelt, dass speziell an die Erfordernisse der Qualitätsüberwachung in Schienenbearbeitungsmaschinen angepasst ist. Das Prüfsystem wird vorgestellt und über erste Erfahrungen aus dem praktischen Einsatz wird berichtet.
Ultrasonic echo and transmission techniques are used in civil engineering on a regular basis. New sensors and data processing techniques have lead to many new applications in the structural investigation as well as quality control. But concrete structures in the nuclear sector have special features and parameters, which pose problems for the methods and instrumentation currently available, e.g. extreme thickness, dense reinforcement, steel liners or special materials. Several innovative ultrasonic techniques have been developed to deal with these issues at least partly in lab experiments and pilot studies. Modern imaging techniques as multi-offset SAFT have been used e. g. to map delaminations. Thick concrete walls have successfully been inspected, partly through a steel liner. Embedded ultrasonic sensors have been designed which will be used in monitoring networks of large concrete structures above and below ground. In addition, sensitive mathematical methods as coda wave interferometry have been successfully evaluated to detect subtle changes in material properties. Examples of measurements and data evaluation are presented.
Indirect UV-absorption spectrometry was shown to be a valuable tool for chemical characterization of functionalized carbon nanotubes (CNTs). It complements data from X-ray photoelectron spectroscopy (XPS) or FTIR analysis since it helps to clarify the type and concentration of functional groups. The principles of indirect application of UV-spectrometry and its mathematical interpretation are discussed. Their facile application, together with their adequate sensitivity and high flexibility, make UV-absorption-based approaches a valuable alternative to fluorescence spectrometry. Here, the approach was applied to the chemical analysis of oxidizing substances on CNTs. For this, pristine CNTs of low but finite oxygen content as well as brominated CNTs were analyzed by reaction in suspension with UV-active thiol reagents and a styrene derivative. It was shown that carefully selected reagents allow differentiation and quantification of bromine and generally oxidizing entities like oxygen. For brominated CNTs, it was shown that physisorbed bromine may dominate the overall bromine content.
Häufig müssen rotierende metallische Bauteile im Betrieb auf das Entstehen rissartiger Fehler überwacht werden. Hierbei besteht im Allgemeinen die Anforderung, trotz extrem schwieriger Umweltbedingungen eine sichere Prüfaussage zu gewährleisten. Es wurden Untersuchungen durchgeführt, inwieweit passive induktive Sensoren in der Lage sind, diese Anforderungen zu erfüllen. Hierzu wurden verschiedene einfache Sensormodelle aufgebaut und an verschiedenen Vergleichsfehlern erprobt. Die Ergebnisse der Untersuchungen werden vorgestellt. Insbesondere die Möglichkeiten und Grenzen dieser einfachen Sensortypen werden herausgearbeitet.
A fiber Bragg grating (FBG) strain patch specially adapted for long-term and high-strain applications has been developed and characterized. The design concept for the patch is based on a glass-fiber reinforced plastic (gfrp) carrier material. The developed concept for the FBG integration into the carrier material was derived from reliable integration procedure of FBG sensors into composite structures. The patches' temperature sensitivity, strain gauge factor, fiber–matrix interface adhesion and fatigue behavior were characterized. As a result, FBG strain patches with linear temperature and strain behavior, as well as excellent fatigue resistance, were developed and can be used as part of a monitoring system for advanced composite materials in aerospace structures or wind turbine power plants.
GMR sensors are widely used in many industrial segments such as information technology, automotive, automation and production, and safety applications. Each area requires an adaption of the sensor arrangement in terms of size adaption and alignment with respect to the field source involved. This paper deals with an analysis of geometric sensor parameters and the arrangement of GMR sensors providing a design roadmap for non-destructive testing (NDT) applications. For this purpose we use an analytical model simulating the magnetic flux leakage (MFL) distribution of surface breaking defects and investigate the flux leakage signal as a function of various sensor parameters. Our calculations show both the influence of sensor length and height and that when detecting the magnetic flux leakage of µm sized defects a gradiometer base line of 250 µm leads to a signal strength loss of less than 10% in comparison with a magnetometer response. To validate the simulation results we finally performed measurements with a GMR magnetometer sensor on a test plate with artificial µm-range cracks. The differences between simulation and measurement are below 6%. We report on the routes for a GMR gradiometer design as a basis for the fabrication of NDT-adapted sensor arrays. The results are also helpful for the use of GMR in other application when it comes to measure positions, lengths, angles or electrical currents.
A unifying review of bioassay-guided fractionation, effect-directed analysis and related techniques
(2012)
The success of modern methods in analytical chemistry sometimes obscures the problem that the ever increasing amount of analytical data does not necessarily give more insight of practical relevance. As alternative approaches, toxicity- and bioactivity-based assays can deliver valuable information about biological effects of complex materials in humans, other species or even ecosystems. However, the observed effects often cannot be clearly assigned to specific chemical compounds. In these cases, the establishment of an unambiguous cause-effect relationship is not possible. Effect-directed analysis tries to interconnect instrumental analytical techniques with a biological/biochemical entity, which identifies or isolates substances of biological relevance. Successful application has been demonstrated in many fields, either as proof-of-principle studies or even for complex samples. This review discusses the different approaches, advantages and limitations and finally shows some practical examples. The broad emergence of effect-directed analytical concepts might lead to a true paradigm shift in analytical chemistry, away from ever growing lists of chemical compounds. The connection of biological effects with the identification and quantification of molecular entities leads to relevant answers to many real life questions.
Several construction and building materials, including wood, glue and coatings, are possible sources of very volatile organic compounds (VVOCs) and volatile organic compounds (VOCs) like formic and acetic acid. Due to very high air tightness and very low air exchange rates in new buildings concentrations of these harmful substances can increase considerably. To minimize the risk, emissions from building products should be identified and quantified. With the common standard method, this means Tenax® sampling followed by thermal desorption and GC-MS analysis, these acids could not be detected sufficiently. The aim oft this study is the comparison of two different methods for the determination of acetic and formic acid. The sampling of method one, which is usually used for identification and quantification of VOCs, is done in accordance with ISO 16000-6 and ISO 16017-1 on Carbotrap® 202 multi-bed thermal desorption tube by subsequent identification and quantification with GC-MS. Method two is based on sampling on 2,4-dinitrophenylhydrazine (DNPH) cartridges, derivatisation, elution, identification and quantification of the derivatives with LC-MS/MS (liquid chromatography mass spectrometry/mass spectrometry).
Combustion of peroxy-fuels
(2011)
The diffusion flames of organic peroxides exhibit quite different characteristics than hydrocarbons. What makes them interesting to study is their fast burning behaviour. As a result the flame temperature enhances and so does the thermal radiation. Due to all these they demand safe handling during processing. However, they can be utilised at several places in different industries where a fuel with fast burning, high temperature and intense radiation are desired. Some of the possibilities to use them as a main or supporting fuel in a wide range of industrial utilities are the major content of this paper.
The use of energetic materials as a main fuel in high temperature process
industries are not known to the scientific community as such. This paper
highlights some of the features and advantages of using organic peroxides
especially di-tert-butyl peroxide (DTBP) in high temperature process industries.
The feasibility of using DTBP as a main or supporting fuel in process industries
have also been justified with the help of Computational Fluid Dynamics (CFD)
simulations. For peroxides requirement of less fuel and air for the same amount
of heat flux has been shown. The resulted emission from the combustion of
DTBP is also discussed.
Triacetone triperoxide (TATP) is a primary explosive, which was used in various terrorist attacks in the past. For the development of biosensors, immunochemical µ-TAS, electronic noses, immunological test kits, or test strips, the availability of antibodies of high quality is crucial. Recently, we presented the successful immunization of mice, based on the design, synthesis, and conjugation of a novel TATP derivative. Here, the long-term immunization of rabbits is shown, which resulted in antibodies of extreme selectivity and more than 1,000 times better affinity in relation to the antibodies from mice. Detection limits below 10 ng L-1 (water) were achieved. The working range covers more than four decades, calculated from a precision profile. The cross-reactivity tests revealed an extraordinary selectivity of the antibodies—not a single compound could be identified as a relevant cross-reactant. The presented immunoreagent might be a major step for the development of highly sensitive and selective TATP detectors particularly for security applications.
Ground penetrating radar (GPR) was used to characterize the frequency-dependent dielectric relaxation phenomena in ordinary Portland cement (OPC) hydration in concrete changing from fresh to hardened state. The study was experimented by measuring the changes of GPR A-scan waveforms over a period of 90 days, and processed the waveforms with short-time Fourier transform (STFT) in joint time-frequency analysis (JTFA) domain rather than a conventional time or frequency domain alone. The signals of the direct wave traveled at the concrete surface and the reflected wave from an embedded steel bar were transformed with STFT, in which the changes of peak frequency over ages were tracked. The peak frequencies were found to increase with ages and the patterns were found to match closely with primarily the well-known OPC hydration process and secondarily, the evaporation effect. The close match is contributed to the simultaneous effects converting free to bound water over time, on both conventional OPC hydration and dielectric relaxation mechanisms.
Digital radiography in the inspection of welded pipes to be installed under deep water offshore gas and oil pipelines, like a presalt in Brazil, in the paper has been investigated. The aim is to use digital radiography for nondestructive testing of welds as it is already in use in the medical, aerospace, security, automotive, and petrochemical sectors. Among the current options, the DDA (Digital Detector Array) is considered as one of the best solutions to replace industrial films, as well as to increase the sensitivity to reduce the inspection cycle time. This paper shows the results of this new technique, comparing it to radiography with industrial films systems. In this paper, 20 test specimens of longitudinal welded pipe joints, specially prepared with artificial defects like cracks, lack of fusion, lack of penetration, and porosities and slag inclusions with varying dimensions and in 06 different base metal wall thicknesses, were tested and a comparison of the techniques was made. These experiments verified the purposed rules for parameter definitions and selections to control the required digital radiographic image quality as described in the draft international standard ISO/DIS 10893-7. This draft is first standard establishing the parameters for digital radiography on weld seam of welded steel pipes for pressure purposes to be used on gas and oil pipelines.
Phosphorus-based flame retardancy mechanisms - Old hat or a starting point for future development?
(2010)
Different kinds of additive and reactive flame retardants containing phosphorus are increasingly successful as halogen-free alternatives for various polymeric materials and applications. Phosphorus can act in the condensed phase by enhancing charring, yielding intumescence, or through inorganic glass formation; and in the gas phase through flame inhibition. Occurrence and efficiency depend, not only on the flame retardant itself, but also on its interaction with pyrolysing polymeric material and additives. Flame retardancy is sensitive to modification of the flame retardant, the use of synergists/adjuvants, and changes to the polymeric material. A detailed understanding facilitates the launch of tailored and targeted development.
The class Dothideomycetes (along with Eurotiomycetes) includes numerous rock-inhabiting fungi (RIF), a group of ascomycetes that tolerates surprisingly well harsh conditions prevailing on rock surfaces. Despite their convergent morphology and physiology, RIF are phylogenetically highly diverse in Dothideomycetes. However, the positions of main groups of RIF in this class remain unclear due to the lack of a strong phylogenetic framework. Moreover, connections between rock-dwelling habit and other lifestyles found in Dothideomycetes such as plant pathogens, saprobes and lichen-forming fungi are still unexplored. Based on multigene phylogenetic analyses, we report that RIF belong to Capnodiales (particularly to the family Teratosphaeriaceae s.l.), Dothideales, Pleosporales, and Myriangiales, as well as some uncharacterised groups with affinities to Dothideomycetes. Moreover, one lineage consisting exclusively of RIF proved to be closely related to Arthoniomycetes, the sister class of Dothideomycetes. The broad phylogenetic amplitude of RIF in Dothideomycetes suggests that total species richness in this class remains underestimated. Composition of some RIF-rich lineages suggests that rock surfaces are reservoirs for plant-associated fungi or saprobes, although other data also agree with rocks as a primary substrate for ancient fungal lineages. According to the current sampling, long distance dispersal seems to be common for RIF. Dothideomycetes lineages comprising lichens also include RIF, suggesting a possible link between rock-dwelling habit and lichenisation.
Shape memory polymers (SMP) belong to the class of stimuli-responsive materials and have generated significant research interest. Their capability to retain an imposed, temporary shape and to recover the initial, permanent shape upon exposure to an external stimulus depends on the "functional determinants", which in simplistic terms, can be divided into structural/morphological and processing/environmental factors. The primary aim of the first part of this review is to reflect the knowledge about these fundamental relationships. In a next step, recent advances in shape memory polymer composites are summarized. In contrast to earlier reviews, studies on the impairment of shape memory properties through various factors, such as aging, compression and hibernation, lubricants, UV light and thermo-mechanical cycling, are extensively reviewed. Apart from summarizing the state-of-the-art in SMP research, recent progress is commented.
The changes in the sonic surface wave velocity of concrete under stress were investigated in this paper. Surface wave velocities at
sonic frequency range were measured on a prismatic concrete specimen undergoing several cycles of uniaxial compression. The
loading was applied (or removed) gradually in predefined small steps (stress-controlled). The surface wave velocity was measured
at every load step during both loading and unloading phases. Acoustic Emission (AE) test was conducted simultaneously to
monitor the microcracking activities at different levels of loading. It was found that the sonic surface wave velocity is highly stress
dependent and the velocity-stress relationship follows a particular trend. The observed trend could be explained by a combination
of acoustoelasticity and microcracking theories, each valid over a certain range of applied stresses. Having measured the velocities
while unloading, when the material suffers no further damage, the effect of stress and damage could be differentiated. The slope
of the velocity-stress curves over the elastic region was calculated for different load cycles. This quantity was normalized to yield a
dimensionless nonlinear parameter. This parameter generally increases with the level of induced damage in concrete.
Die zerstörungsfreie Oberflächenprüfung an verlegten Eisenbahnschienen mit Wirbelstrom hat in den letzten Jahren durch ständige Weiterentwicklung und Verifizierung enorm an Bedeutung gewonnen. Es wurde u.a. angestrebt zuverlässige Planungsgrößen für den Einsatz von Instandhaltungsmaßnahmen zu erhalten, durch deren gezielten Einsatz Risswachstum unterbunden werden kann. Die Ursache für das Wachstum von Rissen in der Schiene liegt in der Materialermüdung des Werkstoffes infolge der Betriebsbelastungen im RadSchiene-Kontakt. Nach einer gewissen Beanspruchungsdauer kommt es an den Kontaktflächen der Fahrkante zu einer Kaltverfestigung des Schienenstahls. Durch fortschreitende Verfestigung des kontaktbeanspruchten Oberflächenbereichs der gehärteten Schicht wird der Werkstoff spröde und es bilden sich feine Risse aus. Die Risse wachsen anfangs unter einem flachen Winkel in das Schieneninnere hinein, neigen dann aber ab einem gewissen Stadium dazu in das Innere des Schienenkopfes abzukippen, was im Extremfall zu einem Schienenbruch führen kann. Diese Rollkontaktermüdungsrisse, auch genannt Head Checks, entstehen bevorzugt in der Fahrkante von bogenäußeren Schienen. Die Anwendung der Wirbelstromprüfung an der Schiene wurde bisher zur Ermittlung der Schädigungstiefe dieser Rollkontaktermüdungsrisse eingesetzt. Das Wirbelstromverfahren besitzt die Eigenschaft, sehr empfindlich auf alle Veränderungen der Materialeigenschaften an der Oberfläche zu reagieren. Daher wurde festgestellt, dass sich neben der Detektion von Rissen auch Fehler wie Eindrückungen oder Schlupfwellen, bis hin zu Materialveränderungen durch Schweißen oder Aufhärtungen in der Schienenoberfläche bestimmen lassen. Die Wirbelstromprüfung besitzt daher das Potenzial, mögliche Orte der Entstehung von Ermüdungsrissen in einem extrem frühzeitigen Stadium nachzuweisen. Ziel ist es, die rissgefährdeten Zonen schon im Zustand der Kaltverfestigung zu identifizieren. Dadurch können sich neue Aspekte für die präventive Schieneninstandhaltung ergeben.
Statistical analysis of tomographic reconstruction algorithms by morphological image characteristics
(2010)
We suggest a procedure for quantitative quality control of tomographic reconstruction algorithms. Our task-oriented evaluation focuses on the correct reproduction of phase boundary length and has thus a clear implication for morphological image analysis of tomographic data. Indirectly the method monitors accurate reproduction of a variety of locally defined critical image features within tomograms such as interface positions and microstructures, debonding, cracks and pores. Tomographic errors of such local nature are neglected if only global integral characteristics such as mean squared deviation are considered for the evaluation of an algorithm. The significance of differences in reconstruction quality between algorithms is assessed using a sample of independent random scenes to be reconstructed. These are generated by a Boolean model and thus exhibit a substantial stochastic variability with respect to image morphology. It is demonstrated that phase boundaries in standard reconstructions by filtered backprojection exhibit substantial errors. In the setting of our simulations, these could be significantly reduced by the use of the innovative reconstruction algorithm DIRECTT.