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Eingeladener Vortrag
- nein (1008)
In dieser Arbeit wurden drei verschiedene Nanomaterialien auf ihre Bindungsfähigkeit zu Proteinen untersucht. Zu Beginn standen dabei die Herstellung stabiler Dispersionen der einzelnen Nanopartikel und die Stabilität der gebildeten Konjugate im Vordergrund. Der Nachweis einer erfolgreichen Konjugatbildung, sprich der Beschichtung von Nanopartikel mit Proteinen, wurde sowohl qualitativ mittels DLS-Messungen als auch über quantitative Protein-Bestimmungen erbracht. Für die Quantifizierung konnten verschiedene Methoden eingesetzt werden. Neben der klassischen Vorgehensweise, welche indirekt über die Quantifizierung von ungebundenem Protein im Überstand erfolgt, konnten ihm Rahmen dieser Arbeit verschiedene direkte Bestimmungsmethoden entwickelt werden. So wurden mittels kolorimetrischer Tests, wie dem BCA-Assay und dem Bradford-Assay, Nanodiamantdispersionen mit Hilfe einer Korrekturwellenlänge vermessen und quantifiziert. Ebenso zum Einsatz kam die Methode der Aminosäureanalytik, welche aufgrund ihrer guten Rückführbarkeit auf Aminosäurestandards Ergebnisse mit hoher Richtigkeit generieren kann und ebenso die Detektion kleiner Proteinmengen möglich macht.
Nach den erfolgten quantitativen Betrachtungen wurden die Protein-beschichteten Nanopartikel auf ihre Anwendbarkeit als Analoga von Virus-like Particles (VLP) bei einer Immunisierung zur Gewinnung von polyklonalen Antikörpern gegen humanes Ceruloplasmin in Kaninchen überprüft. Es konnte mittels ELISA gezeigt werden, dass die Konjugate erfolgreich für die Herstellung von Antikörpern eingesetzt werden können und im zeitlichen Verlauf einer Immunisierung eine Steigerung des Antikörper-Titers zu erreichen ist.
Das Ziel der Arbeit war die Entwicklung einer magnetischen Anreicherungsmethode für eine Bead-basierte Substanzbibliothek zur Identifizierung von Proteinbindern. Im Ramen des Forschungsbelegs wurde bereits eine Anreicherungsmethode für ein Modellsystem einer Peptidbibliothek entwickelt. Das Modellsystem bestand dabei aus zwei verschiedenen Peptiden. Als Positivkontrolle wurde das FLAG-Peptid gewählt, welches selektiv gegen den Anti-FLAG-Antikörper bindet, und ein weiteres Peptid wurde als Negativkontrolle gewählt. Anhand dieses Modellsystems konnte die zuvor entwickelte Anreicherungsmethode von 20.000 auf 1.000.000 Beads vergrößert werden. Hierbei wurde ein Anreicherungsfaktor von 818 und eine gute Wiederfindungsrate von 82% erreicht.
This Special Issue of Fire and Materials brings together a Collection of papers that were presented at the 2016 Interflam conference in the Fire & Facades session along with recent submissions to the Fire and Materials Journal that are very relevant to the Fire and Facades subject. Having attended the Interflam conference, all Fire and Materials Journal editors who attended realised the importance of this topic. We felt it important that this session content would both be reviewed and made available to a wider audience and that it was timely that we featured this increasing important topic in our journal. Accordingly, authors of selected papers were invited to update and extend their papers for journal submission, and other appropriate peer review papers subsequently submitted to the journal were included in the collection.
In order to satisfy the growing requirements towards lightweight design and resource efficiency in modern steel constructions, e.g., mobile cranes and bridges, high-strength steels with typical yield strength ≥ 690 MPa are coming into use to an increasing extent. However, these steels require special treatment in welding. The susceptibility for degradation of the mechanical properties
in the presence of hydrogen increases significantly with increasing yield strength. In case of missing knowledge about how and the amount of hydrogen that is uptaken during welding, hydrogen-assisted cracking (HAC) can be a negative consequence.
Moreover, modern weld technology like the modified spray arc process enables welding of narrower weld seams. In this context,
a reduced number of weld beads, volume, and total heat input are technical and economical benefits. This work presents the influence of welding parameters on the diffusible hydrogen content in both (1) single-pass and (2) multi-layer welds. Different
hydrogen concentrations were detected by varied contact tube distance, wire feed speed, arc length, and varied arc type (transitional
arc and modified spray arc). The results show that all welding parameters have significant influence on the diffusible hydrogen concentration in the single-pass welds. By increasing the number of weld beads in case of multi-layer welding, the
hydrogen concentration has been reduced. Whereby, differences in hydrogen concentrations between both arc types are present.
Powder X-ray diffraction is a time-consuming and challenging task, especially for preparation of sensitive phases like ettringite and calcium-silicate-hydrate (C-S-H) phases. Fine-grained ultrahigh-performance concrete (UHPC) with an average grain size <100 μm could be investigated directly without time-consuming milling. As a proof of concept, small UHPC cylinders with plain surfaces were investigated with a newly designed sample holder. The comparison with conventionally prepared powder shows the feasibility of fast qualitative phase analysis using this approach. As a great benefit, a depth-dependent analysis, as well as a comparison of surface layers and core material, was carried out.
Slags from the nonferrous metals industry have great potential to be used as feedstocks for the production of alkali-activated materials. Until now, however, only very limited information has been available about the structural characteristics of these materials. In the work presented herein, synthetic slags in the CaO–FeOx–SiO2 system, representing typical compositions of Fe-rich slags, and inorganic polymers (IPs) produced from the synthetic slags by activation with alkali Silicate solutions have been studied by means of X-ray absorption near-edge structure (XANES) spectroscopy at the Fe K-edge. The iron in the slags was largely Fe2+, with an average coordination number of approximately 5 for the iron in the amorphous fraction. The increase in average oxidation number after alkali-activation was conceptualized as the consequence of slag dissolution and IP precipitation, and employed to calculate the degrees of reaction of the slags. The degree of reaction of the slags increased with increasing amorphous fraction. The iron in the IPs had an average coordination number of approximately 5; thus, IPs produced from the Fe-rich slags studied here are not Fe-analogs of aluminosilicate geopolymers, but differ significantly in terms of structure from the latter.
Photoelectron spectroscopy
(2018)
Time-resolved phase-contrast microscopy is employed to visualize spatio-temporal thermal transients induced by tight focusing of a single Ti:sapphire fs-laser pulse into a solid dielectric sample. This method relies on the coupling of the refractive index change and the sample temperature through the thermo-optic coefficient dn/dT. The thermal transients are studied on a timescale ranging from 10 ns up to 0.1 ms after laser excitation. Beyond providing direct insights into the laser–matter interaction, analyzing the results obtained also enables quantifying the local thermal diffusivity of the sample on a micrometer scale. Studies conducted in different solid dielectrics, namely amorphous fused silica (a-SiO2), a commercial borosilicate glass (BO33, Schott), and a custom alkaline earth silicate glass (NaSi66), illustrate the applicability of this approach to the investigation of various glassy materials.
Meso-Lactide was polymerized in bulk at 60, 80, and 100 °C by means of three different types of catalysts: dibutyltinsulfides (2,2-dibutyl-2-stanna-1,3-dithiolane and 2,20-dibutyl-2-stanna-1,3-dithiane), dibutyltin derivatives of substituted cate-chols (BuCa, CyCa, and BzCa), and dibutyltin derivatives of2,2 dihydroxybiphenyl (SnBi) and 2,2-dihydroxy-1,10-binaphthyl(SnNa. Only the latter two catalysts were active at 60 °C. The architecture of the resulting polylactides depends very much on the structure of the catalyst and on the temperature. At the lowest temperature (60 °C), SnBi and SnNa mainly yielded even-numbered linear chains, but SnNa also yielded even-numbered cycles at 100 °C and short reaction times. In contrast,BuCa, CyCa, and BzCa mainly yielded odd-numbered cycles, although the same catalysts yielded even-numbered linear chains when benzylalcohol was added.
Quantifizierung der Schädigung von DNA in wässriger Lösung unter direkter Elektronenbestrahlung
(2018)
To cure cancer radiation therapy is used to kill tumor cells.
It is based on radiation induced damage to biomolecules.
Especially DNA damage is of key interest due to its central role in apoptosis and mutation.
Because of the high amount of water in biological tissue, most of the damage is caused by the secondary particles produced by the inelastic scattering of ionizing radiation and water.
A detailed understanding of the underlying molecular processes under physiological conditions is the prerequisite to develop more efficient therapies.
Goal of this work is to quantify the DNA damage caused by ionizing radiation in dependence of the inelastic scattering events and the energy deposit within the microscopic target volume of biological relevance.
The irradiations have to be performed in liquid, under consideration of the chemical environment.
Therefore, a new combination of experiment and Monte-Carlo simulations was developed and tested.
To make it possible to irradiate liquids with electrons within scanning electron microscopes a new sample holder was constructed incorporating an electron transparent nanomembrane.
It makes it possible to irradiate DNA, proteins or cells at different pH, salinity and in the presence of cosolutes.
%The most important results of this work are as follows:
The median lethal dose for a model system of plasmid DNA and water was determined by the combination of experimental data, particle scattering simulations (Geant4-DNA) and diffusion calculations as D0.5=(1.7+-0.3) Gy.
From the convolution of plasmid positions and the spatially resolved energy deposit, as determined by electron scattering simulations, the histogram of the energy deposit within the target volume of the plasmids and the microscopic median lethal energy deposit was calculated as E0.5=6+-4eV.
It could be deduced that on average less than two ionization events are sufficient to cause a single-strand-break.
The relation of single-strand-breaks (SSB) to double-strand-breaks (DSB), which is of importance for microdosimetric modeling, was determined as SSB:DSB = 12:1.
The presented method for the determination of microscopic dose-damage relations was further extended to be applicable for general irradiation experiments.
It becomes independent of the type of primary radiation used, the experimental geometry, and the diffusional properties of the molecules under investigation.
This way different experimental systems with varying, inhomogeneous energy deposit characteristics become comparable with each other, which is not possible when only macroscopic averaged values are taken into account.
In addition, the radiation protection properties of the compatible solute ectoine, as well as its influence on the water properties and biomolecules were investigated.
%In addition, the influence of the compatible solute ectoine on water, biomolecules and its radiation protection properties were investigated.
Raman spectroscopy revealed a concentration dependent increase of the collective water modes in the OH-stretching region, which was found to be independent of the sodium chloride concentration.
Molecular dynamic simulations showed that the zwitterionic properties of ectoine lead to its half-chair conformation.
The hydrogen bonds in the first hydration shell are more stable and have an increased lifetime compared to the bulk water.
Irradiation experiments with DNA in the presence of 1M ectoine revealed an increase of the survival rate by a factor of 1.41 as compared to the absence of ectoine.
The protective properties of ectoine result from the increase of the inelastic scattering probabilities of low energy electrons at the acoustic vibrational modes of water and its properties as OH-radical scavenger.
This was shown by Raman spectroscopy and electron paramagnetic resonance measurements (EPR).
Automatisierungs- und Regelkonzepte für das MSG-Engspaltschweißen - Pendel- und Füllgradregelung
(2018)
Das MSG-Engspaltschweißen eignet sich auf Grund der I-Nahtvorbereitung besonders für das wirtschaftliche Fügen bei hohen Blechdicken über 100 mm und bietet darüber hinaus zusätzliche technologische Vorteile. Für die automatisierte Anwendung des Verfahrens unter Produktionsbedingungen muss dabei die Prozesssicherheit auch für mitunter große Variationen der Spaltbreite entlang der Schweißnaht gesichert bleiben. In erster Linie betrifft dies bei mechanischer Auslenkung der Drahtelektrode die Adaption der Pendelbewegung auf die jeweilige Spaltbreite um eine ausreichende Flankenanbindung zu garantieren. Für die Online-Regelung der Pendelbewegung mittels Lichtbogensensorik wurde eine Methode implementiert die die notwendigen Pendelwinkel an jeder Nahtflanke unabhängig ermittelt und darüber hinaus Fehlstellungen des Brenners sowie Veränderungen des Kontaktrohrabstandes und der Prozessparameter eigenständig kompensiert. Eine Füllgradregelung auf Grundlage optischer Erfassung und Auswertung der Schweißnahtgeometrie wurde zusätzlich eingesetzt um bei veränderlichen Nahtquerschnittsflächen einen vorgegebenen, gleichbleibenden Lagenaufbau zu erzielen.
Bei Monopfahlgründungen von Offshore-Windenergieanlagen wird die Verbindung zwischen Monopfahl und Übergangsstück als geschraubter Ringflansch ausgeführt. Die zunehmende Leistungsfähigkeit der Windenergieanlagen führt zu immer größeren Schnittgrößen in diesem Anschluss. In der Folge erhöhen sich nicht nur die Querschnittsabmessungen, sondern es kommen auch zunehmend größere Schrauben zum Einsatz. Da die einschlägigen Regelwerke zur Bemessung dieser Verbindungen nicht für Schrauben der Größen M64 oder M72 konzipiert wurden, stellt sich die Frage der Übertragbarkeit auf solche Anwendungsfälle.
Im Rahmen des Aufsatzes werden Einflüsse diskutiert, die eine Herabsetzung der Schraubentragfähigkeit verursachen könnten. Diese Einflüsse, vornehmlich geometrische Imperfektionen, werden systematisch untersucht und ergänzend in praxisrelevanten Beispielen bewertet. Die somit gewonnenen Erkenntnisse werden für die abschließende Beurteilung der großen Schrauben in Ringflanschverbindungen herangezogen.
Beschaffenheitsanforderungen an Produkte, die Explosionsschutzanforderungen zu erfüllen haben, werden in Deutschland durch die 9. Verordnung zum Produktsicherheitsgesetz (9. ProdSV, Maschinenverordnung) und speziell für atmosphärische Bedingungen in der 11. Verordnung zum Produktsicherheitsgesetz (11. ProdSV, Explosionsschutzverordnung bis 19.4.2016 bzw. Explosionsschutzprodukteverordnung ab 20.04.2016) geregelt. Wesentlicher Inhalt dieser Verordnungen und der Europäischen Richtlinie 2014/34/EU sind die Begriffsdefinitionen für Geräte, Schutzsysteme und Komponenten, das System der Konformitätsbewertung und die Konformitätserklärung, sowie die grundlegenden Sicherheits- und Gesundheitsanforderungen. Es gilt dabei das Prinzip der Herstellerverantwortung. Der Hersteller eines Produktes dokumentiert die Erfüllung der Richtlinienanforderungen mit seiner Konformitätserklärung und der Kennzeichnung des Produktes mit dem CE-Zeichen.
Beschaffenheitsanforderungen an Produkte, die Explosionsschutzanforderungen zu erfüllen haben, werden in Deutschland durch die 9. Verordnung zum Produktsicherheitsgesetz (9. ProdSV, Maschinenverordnung) und speziell für
atmosphärische Bedingungen in der 11. Verordnung zum Produktsicherheitsgesetz (11. ProdSV, Explosionsschutzverordnung bis 19.4.2016 bzw. Explosionsschutzprodukteverordnung ab
20.04.2016) geregelt. Wesentlicher Inhalt dieser Verordnungen und der Europäischen Richtlinie 2014/34/EU sind die Begriffsdefinitionen für
Geräte, Schutzsysteme und Komponenten, das System der Konformitätsbewertung und die Konformitätserklärung, sowie die grundlegenden Sicherheits- und Gesundheitsanforderungen. Es gilt dabei das Prinzip der Herstellerverantwortung. Der Hersteller eines Produktes dokumentiert die Erfüllung der Richtlinienanforderungen mit seiner Konformitätserklärung und der Kennzeichnung des Produktes mit dem CE-Zeichen.
The Scaled Boundary Finite Element Method (SBFEM) is a semi-analytical method that showed promising results in modelling of guided ultrasonic waves. Efficiency and a low computational cost of the method are achieved by the discretisation of the boundary of a computational domain only, whereas for the domain itself the analytical solution is used. By means of the SBFEM different types of defects, e.g. fatigue cracks, pores, delamination, corrosion, integrated into a structure consisting of anisotropic and isotropic materials can be modelled.
In this contribution, the SBFEM is used to analyse the propagation of guided waves in a structure consisting of an isotropic metal bonded to anisotropic carbon fibre reinforced material. The method allowed to identify appropriate wave types (modes) and to analyse their interaction with different defects. Obtained results will be used to develop a structural health monitoring system for composite pressure vessels used in automotive industry.
The hydrogen tightness of high-pressure hydrogen storage is a Basic criterion for long-term storage. The H2 permeation coefficients of epoxy resin and a glass lacquer were determined to enable the geometric optimization of a glass capillary storage. It was found that the curing conditions have no significant influence on the H2 permeation coefficient of resin.
The H2 permeation coefficient of epoxy resin is only about three orders of Magnitude greater than that of borosilicate glass. This suggests that the initial pressure of 700 bar takes about 2.5 years to be halved in capillary array storage. Therefore, a high-pressure hydrogen storage tank based on glass capillaries is ideally suited for long-term storage in mobile applications.
Fachinformationssystem Datenbank GEFAHRGUT - Jetzt auch Hilfe bei der Kennzeichnung der Umweltgefahr
(2018)
Um Gefahrgutumschließungen richtig kennzeichnen zu können ist es erforderlich zu wissen, ob ein Stoff umweltgefährdende Eigenschaften hat. Als Informationsquelle hierfür kann sowohl die Rechercheanwendung der Datenbank GEFAHRGUT als auch die Daten des Gefahrgutdatenservices im BAM-Nummern-System als auch im UN-Nummern-Systems verwendet werden.
Polyesters with 9,10-dihydro-9-oxy-10-phosphaphenanthrene-10-oxide-containing comonomers are synthesized aiming to improve the flame retardancy of aliphatic polyesters such as poly(butylene succinate) and poly(butylene sebacate). The influence of the chemical structure on the thermal decomposition and pyrolysis is examined using a combination of thermogravimetric analysis (TGA), TGA-Fourier transform infrared (FTIR) spectroscopy, pyrolysis-gas chromatography/mass spectrometry, and microscale combustion flow calorimetry. Thermal decomposition pathways are derived and used to select suitable candidates as flame retardants for PBS. The fire behavior of the selected polymers is evaluated by forced-flaming combustion in a cone calorimeter. The materials show two modes of action for flame retardancy: strong flame inhibition due to the release of a variety of molecules combined with charring in the solid state.
The aldoximes C11H9NO (I) and C15H11NO (II), synthesized in ca 90%yield, by
treatment of 1-naphthaldehyde or phenanthrene-9-carbaldehyde, respectively,
with hydroxylamine hydrochloride and sodium carbonate, have been characterized
by IR, 1H, 13C and DEPT-135 NMR spectroscopies, and also by singlecrystal
X-ray diffraction analysis. The molecules of (I) and (II) are
conformationally similar, with the aldoxime substituent groups lying outside
the planes of the naphthalene or phenanthrene rings, forming dihedral angles
with them of 23.9 (4) and 27.9 (6)°, respectively. The crystal structures of both
(I) and (II) are similar with a single intermolecular O—H...N hydrogenbonding
interaction, giving rise to the formation of one-dimensional polymeric
chains extending along the 21 (b) screw axes in each.
Calcium cobaltite is one of the most promising oxide p-type thermoelectric materials. The solid-state reaction (or calcination, respectively), which is well known for large-scale powder synthesis of functional materials, can also be used for the synthesis of thermoelectric oxides. There are various calcination routines in literature for Ca3Co4O9 powder synthesis, but no systematic study has been done on the influence of calcination procedure on thermoelectric properties. Therefore, the influence of calcination conditions on the Seebeck coefficient and the electrical conductivity was studied by modifying calcination temperature, dwell time, particle size of raw materials and number of calcination cycles. This study shows that elevated temperatures, longer dwell times, or repeated calcinations during powder synthesis do not improve but deteriorate the thermoelectric properties of calcium cobaltite. Diffusion during calcination leads to idiomorphic grain growth, which lowers the driving force for sintering of the calcined powder. A lower driving force for sintering reduces the densification. The electrical conductivity increases linearly with densification. The calcination procedure barely influences the Seebeck coefficient. The calcination procedure has no influence on the phase formation of the sintered specimens.
Recycling-Düngemittel auf Basis von sekundären Ressourcen (Gülle, Gärreste, Klärschlamm, Tiermehl etc.) gewinnen in den letzten Jahren zunehmend an Bedeutung in der Landwirtschaft. Die in den Recycling-Düngemitteln enthaltenen P-Spezies weichen oft stark von denen in konventionell hergestellten Düngemitteln aus Rohphosphat ab, zudem enthalten Recyclingdünger oft mehrere verschiedene P-Formen. Die Pflanzenverfügbarkeit des P in ist ganz wesentlich von der enthaltenen P-Form abhängig. Derzeit gibt es außer zeitaufwendigen und kostspieligen Gefäß- und Feldversuchen keine zufriedenstellende Testmethode zur Analyse der P-Pflanzenverfügbarkeit von unterschiedlichen Recycling P-Düngemitteln. Die im europäischen Düngemittelrecht normierten chemischen Extraktionsmethoden (Wasser, Zitronensäure, Ameisensäure, neutral Ammoniumcitrat etc.) zeigen oftmals keine oder nur sehr geringe Korrelation zu der P-Aufnahme von Pflanzen in Gefäßversuchen mit Recycling-Düngemitteln (Kratz et al. 2010, Steckenmesser et al. 2017, Vogel et al. 2017). Eine grundlegende Schwäche chemischer Extraktionsmethoden liegt darin, dass es sich dabei um statische Methoden handelt, die nicht in der Lage sind, die im System Boden/Düngemittel-Bodenlösung-Pflanze stattfindenden dynamischen Prozesse wie P-Freisetzung und Entzug durch die Pflanzenwurzeln abzubilden.
Einen Lösungsansatz bieten hier sog. P-Senken-Methoden. Bereits in den 1950er Jahren wurden erstmals P-Senken zur Analyse des Boden-P angewendet (Chardon et al. 1996). In den darauffolgenden Jahrzehnten wurden verschiedene P-Senken auf der Basis von Eisenoxid-Papier entwickelt (Chardon et al. 1996). Jedoch konnten diese Ansätze auch nur begrenzt zur Bestimmung der P-Pflanzenverfügbarkeit des Boden-P eingesetzt werden. Mitte der 1990er Jahre wurde die DGT (engl. diffusive gradients in thin films) Methode entwickelt (Zhang et al. 1998). Bei der DGT Methode diffundiert P aus der Bodenlösung des angefeuchteten Bodens durch einen Membranfilter und die Diffusionsschicht und wird anschließend an einer Bindungsschicht absorbiert. Durch den Diffusionsgradienten wird das Gleichgewicht in der Bodenlösung permanent gestört, wodurch auch labiles P im Boden gelöst wird. Die stetige Entnahme von P aus der Bodenlösung über die Diffusions-/Bindungsschicht simuliert dabei den Entzug von P durch die Pflanzenwurzel. Die an die Bindungsschicht adsorbierte Menge an P korreliert stark mit der P-Aufnahme von Pflanzen (u.a. Mason et al. 2005, 2013; Menzies et al. 2005, Six et al. 2012). Im Gegensatz zu chemischen Extraktionsmethoden werden bei der DGT Methode Mischungen an Düngemittel und Boden für mehrere Tage inkubiert (Vogel et al. 2017; Duboc et al. 2017), da ansonsten wasserlösliche P-Dünger den DGT Adsorber sättigen und wasserunlösliche P-Dünger unterschätzt werden. Ein bis zwei Wochen Inkubation sind ausreichend, damit sich pflanzenverfügbares P in die Mischungen bildet.
In letzter Zeit haben verschiedene Forschungsgruppen gezeigt, dass die DGT Methode auch eine sehr gute Korrelation mit der Pflanzenverfügbarkeit verschiedener Typen von (Recycling-)P-Düngemitteln aufweist (Vogel et al. 2017; Duboc et al. 2017; Foereid 2017; Haarstad and Bavor 2017; Lemming et al. 2017). Bei Gefäßversuchen mit verschiedenen Recycling P-Düngemitteln konnte die DGT Methode den Ertrag bzw. die P-Aufnahme von Mais deutlich besser vorhersagen als herkömmliche chemische Extraktionsmethoden (Vogel et al. 2017; Duboc et al. 2017).
Daher kann die DGT Methode im Vorfeld der Zulassung von neuen Düngermitteltypen als zuverlässige und robuste Methode zum Screening von Produktvarianten eines Düngemittelherstellers verwendet werden. Um dieses Messverfahren im Rahmen des Düngemittelrechts als Bewertungsinstrument für die Abschätzung der Pflanzenverfügbarkeit unterschiedlicher Düngemittel zu verwenden, muss es allerdings zunächst standardisiert werden. Zu diesem Zweck bietet sich der Einsatz eines „standardisierten“ Bodens bzw. Bodenrezepts an. Zur Kalibrierung der Methode im jeweiligen Labor könnten auch chemisch definierte P-Verbindungen mit bekannter Löslichkeit/Pflanzenverfügbarkeit als Referenz-substanzen verwendet werden.
Der Vortrag widmet sich der „ELLIPSOMETRISCHE KLASSIFIZIERUNG VON KOHLENSTOFFSCHICHTEN“ und beschreibt die Punkte: 1. Anwendungen Kohlenstoffschichten–Carbon–based films (DLC) aus dem Vortrag N. Ohtakeet. al. (ISO TC 107, Tokyo 2017),2. Präparation der Kohlenstoffschichten für ISO TC 107 Ringversuch aus Vortrag M. Hiratsuka et. al. (ISO TC 107, Tokyo 2017), 3. Ellipsometrische Charakterisierung von Kohlenstoffschichten, Ergebnisse des Ringversuchs (ISO TC 107, Tokyo 2017) Vortrag Beck et. al. und 4.Deutsche Normungsaktivitäten national/international zur Ellipsometrie DIN NA 062-01-061 (DIN 50989-1)/TC 107 (PWI DE)“ im Einzelnen.
Partial penetration welding with fiber laser on 20mm thick plates was carried out in horizontal position to study the role of secondary heating in modeling of high power fiber laser welding. Experiments were carried out using 18.8kW laser with 1.5 m/min welding speed at Ar assist gas flow rates of 0, 17, 29, and 40 l/min, all four cases show similar bead shape with bright emission of vapor plume. Numerical simulations were performed using volume of fluid method by considering three different models as models A–C. Model A considers only Fresnel reflection inside the keyhole using real time tracking of free surface. Model B considers vapor recondensation flux inside keyhole along with model A. Finally, model C is used, which considers vapor plume heating at 4100K temperature along with models A B. Secondary heating by recondensation and vapor plume is vital in modeling of high power fiber laser welding; especially, the upper part of the bead is more influenced due to secondary heating. Tungsten particles are also used to visualize the flow pattern of melt pool.
Performing mechanical tests at high temperatures is a nontrivial issue: Compared to room temperature testing, additional phenomena like time-dependent Deformation processes and oxidation effects raise the complexity of the material’s response, while more sophisticated test setups and additional control parameters increase the number of potential sources of error. To a large extent, these complications can be overcome by carefully following all recommendations given in the respective high temperature testing standards, but more comprehensive background information helps to identify points of specific importance in particular test campaigns. In this chapter, an overview is given on general high temperature testing issues like the appropriate choice of experimental equipment and key aspects of temperature measurement. In subsequent sections, the major static and dynamic high temperature test methods are reviewed and their Special features, as compared to testing at room temperature, are highlighted based on example data sets. Influences of specimen size and environmental effects are shortly outlined in a concluding section. In the whole chapter, a focus is set on testing of “classical” metallic high temperature materials, but many considerations are equally valid for testing of intermetallics, composites, and high temperature ceramics.
During the past few years significantly increasing research activities in the field of laser-induced periodic surface structures (LIPSS, ripples) have been reported since the generation of LIPSS in a single-step process provides a simple way of surface nanostructuring towards a control of optical, mechanical or chemical surface properties. In this contribution the current research state in this field is reviewed. The formation of LIPSS upon irradiation of metals, semiconductors and dielectrics by multiple linearly polarized Ti:sapphire fs-laser pulses (30-150 fs) is studied experimentally and theoretically. Different types of LIPSS with periods even below 100 nm can be generated. Their dynamics and formation mechanisms are analyzed and identified in ultrafast optical experiments. Complementing theoretical calculations of the laser-induced carrier dynamics address transient changes of the optical properties of the irradiated materials and reveal the importance of surface plasmon polaritons in the early stage of LIPSS formation. Various applications of these nanostructures are outlined.
One of the holy grails in chemistry is to reconstruct some of life’s functions with synthetic materials. In this contribution, we demonstrate that “simple” macromolecular architectures such as dendritic amphiphiles, Janus dendrimers, thermoresponsive and hybrid organic-inorganic (co)polymers enable to mimic some of the functions of proteins for biomineralization, natural bactericides, biological membranes or the stimuli-responsive cytoskeleton.
Contrast-variation small-angle neutron scattering (CV-SANS), small-angle X-ray scattering (SAXS), nuclear magnetic resonance (NMR) measurements of diffusion and isothermal titration calorimetry (ITC) are used to gain insight into the aggregation of an alkyl–C60 derivative, molecule 1, in n-hexane, n-decane and toluene as a function of concentration and temperature. Results point to an associative mechanism of aggregation similar to other commonly associating molecules, including non-ionic surfactants or asphaltenes in non-aqueous solvents. Little aggregation is detected in toluene, but small micelle-like structures form in n-alkane solvents, which have a C60-rich core and alkyl-rich shell. The greatest aggregation extent is found in n-hexane, and at 0.1 M the micelles of 1 comprise around 6 molecules at 25 °C. These micelles become smaller when the concentration is lowered, or if the solvent is changed to n-decane. The solution structure is also affected by temperature, with a slightly larger aggregation extent at 10 °C than at 25 °C. At higher concentrations, for example in solutions of 1 above 0.3 M in n-decane, a bicontinuous network becomes apparent. Overall, these findings aid our understanding of the factors driving the assembly of alkyl–π-conjugated hydrophobic amphiphiles such as 1 in solution and thereby represent a step towards the ultimate goal of exploiting this phenomenon to form materials with well-defined order.
Distributed Fibre Optic Sensing for Monitoring and Testing of Industrial and Civil Infrastructures
(2018)
Fibre optic sensors enable the gathering of sensory information in environments where conventional sensors fail or simply can not be utilised. Their small size enables their use in confined spaces as well as their embedding or integration in components, structures or composite materials while offering, depending on the approach, high sensitivity, very high spatial resolution and, especially, the possibility to detect or measure physical quantities in a distributed way, meaning spatially continuous sensing over very long distances.
Those distributed fibre optic sensors (DFOS) provide access to sensing information from different locations along the sensing fibre without the need for technologically challenging multiplexing of many point sensors and the subsequent sensor data fusion. In this way, DFOS are excellently suited as smart sensors for monitoring or testing purposes as the spatially distributed sensing data make available spatially resolved measurand profiles without a gap. Furthermore, the possible embedding or integration of DFOS could facilitate the development of smart structures or smart components. In particular distributed vibration sensing (DVS) and distributed temperature sensing (DTS) are also ideally suited for condition monitoring of machinery, industrial installations or extensive infrastructure, also, on-line real-time assembly or component testing in production lines, e.g. for quality control, is possible.
In this talk, we will shortly outline the underlying principles of some fibre optic sensing approaches, explain their fundamental differences in mode of operation and performance, and discuss their applicability and limitations. Moreover, we will report on a subset of current and previous applied research projects at BAM, investigating different areas of use for distributed fibre optic sensors in particular.
A novel method to generalize kinetic data of viscous crack healing in glasses is proposed. The method assumes that crack healing progress is proportional to the healing time, t, and indirect proportional to viscosity, n. This way, crack length and crack width data, normalized to the initial crack length and plotted versus t/n, allow to compare crack healing progress for different cracks and healing temperatures in a master curve. Crack healing experiments conducted in this study demonstrate the applicability of this method for a commercial microscope slide glass.
Das bislang zur Vermeidung unzulässiger Wurzelüberhöhungen beim Laserstrahlschweißen von Aluminiumlegierungen bzw. austenitischem Stahl eingesetzte Verfahren der elektromagnetischen Schmelzbadstütze konnte innerhalb der vorliegenden Untersuchung erfolgreich zur Kompensation des hydrostatischen Druckes von ferromagnetischen Stählen übertragen werden. Es wurden dabei Laserstrahlschweißversuche in PA-Position an bis zu 20 mm dickem Duplexstahl 1.4462 sowie Baustahl S235JR durchgeführt. Unter konstanten Schweißparametern wurden Durchschweißungen generiert. Dem hydrostatischen Druck wurde unter Verwendung der Technologie zur elektromagnetischen Schmelzbadunterstützung durch Variation der Oszillationsfrequenz und der AC-Leistung des Magnetsystems entgegengewirkt.
Zunächst konzentrierten sich die Versuche auf den Duplexstahl 1.4462, welcher jeweils aus 50 % Ferrit und Austenit besteht. Hierbei konnte festgestellt werden, dass zur idealen Kompensation von 15 mm bei einer Frequenz von 1,7 kHz eine AC-Leistung von 1,6 kW erforderlich ist, die Schweißnähte aber bereits bei einer AC-Leistung von ca. 0,8 kW in die Bewertungsgruppe B der DIN EN ISO 13919-1:1996-09 eingeordent werden können. Zur idealen Kompensation des hydrostatischen Druckes bei 20 mm dickem Duplexstahl war eine um 20 % höhere AC-Leistung notwendig. Im Anschluss an die Versuche mit dem Duplexstahl wurden die Untersuchungen auf bis zu 20 mm dicke Proben aus Baustahl S235JR erweitert. Für 15 mm konnten die Schweißnähte bei einer Frequenz von 1,7 kHz ab einer AC-Leistung von 1,3 kW in die Bewertungsgruppe B eingeordnet werden. Zur idealen Kompensation von 20 mm dickem Baustahl war eine AC-Leistung von 1,6 kW bei einer Frequenz von 636 Hz nötig. Mit steigender AC-Leistung konnte in allen Versuchsreihen eine sukzessive Verringerung
der Wurzelüberhöhung demonstriert werden.
Proline has been widely used for various cocrystallization applications, including pharmaceutical cocrystals. Combining enantiopure and racemic flurbiprofen and proline, we discovered 18 new crystal structures. Liquid-assisted grinding proved highly efficient to explore all the variety of crystal forms. A unique combination of stateof-the-art characterization techniques, comprising variable temperature in situ X-ray diffraction and in situ ball-milling, along with other physicochemical methods and density functional theory calculations, was indispensable for identifying all the phases. Analyzing the results of in situ ball-milling, we established a stepwise mechanism for the formation of several 1:1 cocrystals via an intermediate 2:1 phase. The nature of the solvent in liquidassisted grinding was found to significantly affect the reaction rate and, in some cases, the reaction pathway.
We demonstrate ultrafast soliton-based nonlinear balancing of dual-core asymmetry in highly nonlinear photonic crystal fiber at sub-nanojoule pulse energy level. The effect of fiber asymmetry was studied experimentally by selective excitation and monitoring of individual fiber cores at different wavelengths between 1500 nm and 1800 nm. Higher energy transfer rate to non-excited core was observed in the case of fast core excitation due to nonlinear asymmetry balancing of temporal solitons, which was confirmed by the dedicated numerical simulations based on the coupled generalized nonlinear Schrödinger equations. Moreover, the simulation results correspond qualitatively with the experimentally acquired dependences of the output dual-core extinction Ratio on excitation energy and wavelength. In the case of 1800 nm fast core excitation, narrow band spectral intensity switching between the output channels was registered with contrast of 23 dB. The switching was achieved by the change of the excitation pulse energy in sub-nanojoule region. The performed detailed analysis of the nonlinear balancing of dual-core asymmetry in solitonic propagation regime opens new perspectives for the development of ultrafast nonlinear all-optical switching devices.
We present an in situ PXRD investigation of the mechanochemical cocrystal formation of pyrazinamide with pimelic acid in two milling jar materials. DFT calculations of the two synthesized polymorphs suggest that the relative stability is based on a conformation change of pyrazinamide in the cocrystal.
High-Amplitude Surge of a Pitching Airfoil: Complementary Wind- and Water-Tunnel Measurements
(2018)
RECENT interest in gust response, rotorcraft forward flight and wind energy, among other applications, has focused on streamwise oscillations of nominally two-dimensional airfoils in attached and separated flows. The airfoil may be simultaneously held at constant incidence or execute some maneuver, such as pitch.
The relative freestream is spatially uniform but temporally unsteady, and this can be accomplished in a ground-test facility in two ways. The first method is to vary the output of the prime mover, such as the rotational speed of the impeller or the blower driving a wind tunnel, or (alternatively) to vary the pressure drop in the tunnel, thereby varying the flow speed in the test section, despite nominally constant primemover revolutions per minute. The second method is used to keep the tunnel’s operating speed constant, as well as to move the test article in the streamwise direction, fore and aft (for example, via an electric linear motor), such that the relative freestream speed felt by the test article varies according to some waveform. Typically, the latter approach is chosen in water tunnels, where there is too much tunnel-circuit inertia to vary the flow speed directly but where the usually low tunnel test section flow speeds enable large excursions in the relative freestream by oscillation of the test article. In fact, outright reverse flow is possible by moving the test article in the laboratory frame at a higher speed than the water-tunnel flow speed. In either case, a sinusoidal relative-speed waveform is the most intuitively realizable, and this can be combined with similar oscillations in the airfoil incidence angle or other kinematics. Although the two methods of realizing streamwise oscillations are mechanically distinct, experimental comparisons between an oscillating test article in a water tunnel and a stationary test article in a wind tunnel with a louvermechanismhave demonstrated agreement in themeasured lift and drag histories. Such experimentswere performed by Granlund et al. for a 10% freestream amplitude oscillation and fixed airfoil incidence, comparing a free-surface water tunnel and a closed-circuit wind tunnel. After buoyancy was subtracted from the wind-tunnel data (resulting from the louver pressure drop) and the model inertia subtracted from the water-tunnel data (resulting from acceleration of the test article), the remaining lift and drag histories matched well at the low freestream oscillation amplitude regime. The work of Granlund et al. was later extended to high-advance-ratio streamwise oscillations of 50% amplitude by Greenblatt et al., where the aerodynamic histories of the water-tunnel and wind-tunnel facilities were compared in combined pitch and freestreamoscillations (governed by relative pitch phase), pure pitch oscillations, and purely freestream oscillations. Agreement between the two facilities’ data for fixed-incidence streamwise oscillations was reasonably good, and in fact, better than agreement in just the static lift and drag, evidently owing to differences in blockage and model-support systems. Additionally, Greenblatt et al. determined there was no strong coupling between simultaneous freestream oscillations and pitch oscillations on resultant lift and moment coefficients.
This is the first time that PE frits were used to quantify sulfur in copper and its alloys by isotope dilution combined with LA-ICP-MS: an alternative approach for sample preparation. The following properties of the PE frit meet the requirements for isotope dilution LA-ICPMS: porous material, thermo plastic (melting point >100°C), chemical resistance (nitric acid >70%) and high adsorption efficiency. The breakthrough, however, as a support material, especially when comparing the PE frit with other materials such gelatin or sodium silicate is the low blank, which is only two times of the gas flow blank (2.3-4.0 x 10⁴ cps). Additionally, the porosity of the frit was considered, as it directly affects the adsorption efficiency for the sample solution, which is present in the cavities of the frit.
Adsorption efficiency was studied by depositing sulfur standards with varying sulfur amounts (0, 2, 5, 10, 20, 40 and 80 µg S) on the frits. The remaining sulfur which was not absorbed by the frit was rinsed off and was measured by ICP-MS. This indirect method shows that more than 99.5 % of the loaded sulfur was absorbed by the frit. Such high absorption efficiency is completely sufficient for a support material to be used in LA-ICP-IDMS. The so prepared frits with increasing sulfur amount were measured by LA-ICP-MS showing a good linearity between 0 µg S and 40 µg S with a correlation coefficient r2 of 0.9987 and sensitivity of 3.4x10⁴ cps µgˉ¹ for 32S.
Three copper reference materials produced by BAM were selected to develop and validate the LA-ICP-IDMS procedure. The IDMS technique was applied to these samples as follows: the samples were spiked, dissolved, digested and then the digest was adsorbed on the frits.
A laser-based bottom-up technique for the fabrication of Cu(In,Ga)Se2 (CIGSe) micro solar cells is presented.
We use femtosecond laser-induced forward transfer (LIFT) to transport a metallic precursor composed of copper, indium, and gallium onto a molybdenum back contact layer on a glass substrate. A CIGSe absorber forms by subsequent selenization. An array of micro absorbers with defined spacing is fabricated to solar cells and characterized under concentrated light illumination. The solar cell array exhibited a conversion efficiency of 1.4‰ at 1 sun as well as a significant efficiency enhancement of 68% rel. under 20-fold concentration. This work demonstrates the possibility of directly grown micrometer-sized solar cells based on chalcogenide absorber layers, enabling effective material usage.
Quantitative analysis of complex proteins is a challenging task in modern bioanalytical chemistry. Commonly available isotope labels are still suffering from limitations and drawbacks, whereas new metal labels open numerous possibilities in mass spectrometric analyses. In this work, we have developed a newmetal labeling strategy to tag glycan structures of proteins, more particularly antibodies. The oligosaccharide glycans were selectively trimmed to the last N-acetylglucosamine to which an artificial azide containing galactose residue was bound. This azide can be used for subsequent cycloaddition of an alkyne. Therefore, we developed a lanthanide-containing macrocyclic reagent to selectively connect to this azido galactose. In summary, the glycan structures of an antibody can be labeled with a metal functionality using this approach. Furthermore, the functionality of the antibodies can be fully maintained by labeling the Fc glycans instead of using labeling reagents that target amino or thiol groups. This approach enables the possibility of using elemental, besides molecular mass spectrometry, for quantitative analyses or imaging experiments of antibodies in complex biological samples.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
Combining experiments and all-atom molecular dynamics simulations, we study the conformational behavior of polyacrylamide (PAM) in aqueous alcohol mixtures over a wide range of temperatures. This study Shows that even when the microscopic interaction is dictated by hydrogen bonding, unlike its counterparts that present a lower critical solution temperature (LCST), PAM shows a counterintuitive tunable upper critical solution temperature (UCST)-type phase transition in water/alcohol mixtures that was not reported before. The Phase transition temperature was found to be tunable between 4 and 60 1C by the type and concentration of alcohol in the mixture as well as by the solution concentration and molecular weight of the polymer. In addition, molecular dynamics simulations confirmed a UCST-like behaviour of the PAM in aqueous alcoholic solutions.
Additionally, it was observed that the PAM is more swollen in pure alcohol solutions than in 80% alcoholic solutions due to y-like behaviour. Additionally, in the globular state, the size of the aggregates was found to increase with increasing solvent hydrophobicity and polymer concentration of the solutions. Above ist Phase transition temperature, PAM might be present as individual polymer chains in the coil state (r10 nm). As PAM is a widespread polymer in many biomedical applications (gel electrophoresis, etc.), this finding could be of high relevance for many more practical applications in high performance pharmaceuticals and/or sensors.
Pulse thermography (PT) has proven to be a valuable non-destructive testing method to identify and quantify defects in fiber-reinforced polymers. To perform a quantitative defect characterization, the heat diffusion within the material as well as the material parameters must be known. The heterogeneous material structure of glass fiber-reinforced polymers (GFRP) as well as the semitransparency of the material for optical excitation sources of PT is still challenging. For homogeneous semitransparent materials, 1D analytical models describing the temperature distribution are available.
Here, we present an analytical approach to model PT for laterally inhomogeneous semitransparent materials.We show the validity of the model by considering different configurations of the optical heating source, the IR camera, and the differently coated GFRP sample. The model considers the lateral inhomogeneity of the semitransparency by an additional absorption coefficient. It includes additional effects such as thermal losses at the samples surfaces, multilayer systems with thermal contact resistance, and a finite duration of the heating pulse. By using a sufficient complexity of the analytical model, similar values of the material parameters were found for all six investigated configurations by numerical fitting.
A key limitation of the most constitutive models that reproduce a Degradation of quasi-brittle materials is that they generally do not address issues related to fatigue. One reason is the huge computational costs to resolve each load cycle on the structural level. The goal of this paper is the development of a temporal Integration scheme, which significantly increases the computational efficiency of the finite element method in comparison to conventional temporal integrations.
The essential constituent of the fatigue model is an implicit gradient-enhanced formulation of the damage rate. The evolution of the field variables is computed as amultiscale Fourier series in time.On a microchronological scale attributed to single cycles, the initial boundary value problem is approximated by linear BVPs with respect to the Fourier coefficients. Using the adaptive cycle jump concept, the obtained damage rates are transferred to a coarsermacrochronological scale associated with the duration of material deterioration. The performance of the developedmethod is hence improved due to an efficient numerical treatment of the microchronological problem in combination with the cycle jump technique on the macrochronological scale. Validation examples demonstrate the convergence of the obtained solutions to the reference simulations while significantly reducing the computational costs.
Analytical flaw assessment
(2018)
The paper provides a review on analytical flaw assessment methods with the focus on fracture under monotonic loading and fatigue crack propagation. The first topic comprises linear elastic as well as elastic-plastic fracture mechanics approaches. It essentially follows their historical development. Topics which are separately discussed are reference/Limit loads, the treatment of secondary stresses, strength mismatch, constraint, unstable crack propagation (monotonic R-curve analyses) and statistical aspects. With respect to fatigue crack propagation the analytical treatment of crack closure and constraint and the Determination of the cyclic elastic-plastic crack driving force is discussed. Finally, cyclic Rcurve analyses are briefly addressed.