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- Quantitative NMR-Spektroskopie (4)
- qNMR (4)
- Impact (3)
- Reaction monitoring (3)
- Stress wave propagation (3)
- Degradation (2)
- Electron backscatter diffraction (2)
- Fatigue (2)
- Mesoscale (2)
- Metrologie (2)
Eingeladener Vortrag
- nein (73)
Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion beim Schweißen höherfester Feinkornbaustähle mit modifiziertem Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
Due to the large quantities of construction and demolition waste (CDW) in Europe, its reuse or recycling is of particular importance. Although several countries already recycle high amounts of CDW, the use as secondary raw materials is often limited by inferior building material properties. Specific characteristics, like high porosity and low density are caused by hardened cement paste in crushed concrete and the content of mortar and plaster in brick debris. Impurities like wood or gypsum and also harmful substances like organic pollutants may be a major problem for a reuse and should be minimized. Therefore unwanted materials and impairing substances have to be separated from the secondary building material stream. This can be done during the demolition process by using techniques for selective dismantling or during the subsequent treatment of the resulting rubble. Since almost all processing steps are associated with environmental impacts, the benefits of saving natural resources by applying secondary building materials should be weighed carefully. An environmental performance evaluation was undertaken to assess different techniques for reducing gypsum in recycled concrete aggregates, aiming at a minimization of elutable sulfates. These results were compared to the environmental impacts of the extraction of natural aggregates for concrete.
In this work an approach for smoothing the oscillations of normal contact is presented. On the other side a higher order time discretization scheme in association with a higher order spatial discretization, like the spectral element method, is used. The contact constraints are reformulated in order to get an explicit equation for the motion.
In this work an approach for smoothing the oscillations of normal impact is presented. In addition, a higher order time discretization scheme in association with a higher order spatial discretization, like the spectral element method, is investigated regarding its convergence rates.
This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.
The presentation gives an overview about mechanical and thermal testing of packages and containers for radioactive material in Germany. The test facilities of BAM and the main measurement methods are described followed by testing of containers (prototype, full-scale, reduced scale) as well as components and specimens.
The concreting of prefabricated concrete structures can lead to insufficient bonding or even to remaining cavities. Honeycombs (aggregate clusters without cement) represent potential weakening of the structure and need to be detected non-destructively. In our study we tested the capability of ground penetrating radar (GPR) techniques for this purpose. We applied GPR in reflection mode and zero-offset profiling (ZOP) transmission mode on a precast concrete twin wall with built-in honeycombs. GPR measurements were performed as two channel measurement with ground coupled antennas with centre frequencies of 1.5 GHz and 2.6 GHz mounted to an automated scanner system.
Our findings show that ZOP transmission measurements are a more efficient method to detect voids in reinforced concrete structures compared to reflection mode measurements. This holds for both the effort needed for the measurement and the evaluation as well as the validity of the data. Honeycombs (basically representing voids) are usually characterized by strongly reduced amplitudes and earlier arrivals of the transmitted wave.
Abfallgebinde, die im Endlager Konrad eingelagert werden sollen, müssen die Anforderungen und Kriterien erfüllen, die in den Endlagerungsbedingungen (SE-IB-29/08-Rev-1) und in der Produktkontrolle (SE-IB-30/08-Rev-1) festgelegt sind. Die Qualifizierung der Abfallbehälter erfolgt auf dieser Grundlage in Form von Bauartprüfungen, die von der Bundesanstalt für Materialforschung und -prüfung (BAM) im Auftrag des Bundesamtes für Strahlen-schutz (BfS) durchgeführt werden. Darüber hinaus sind die im Hinblick auf Behälterbauartprüfungen relevanten Nebenbestimmungen aus dem Planfeststellungsbeschluss für das Endlager Konrad zu berücksichtigen. Zur besseren Anwendbarkeit werden diese Nebenbestimmungen in die Endlagerungsbedingungen und die Pro-duktkontrolle eingearbeitet. Begleitend ist als Hilfestellung für die Abfallablieferer und Behälterhersteller ein Leit-faden geplant, der praktikable Nachweisstrategien aufzeigt und, soweit erforderlich, Hintergrundinformationen zu den Spezifikationen der Regelwerke liefert. Die BAM ist vom BfS beauftragt, hierfür Vorschläge zu entwickeln und Empfehlungen abzugeben.
The special design of buildings, constructed for nuclear power plants is a particular challenge for the nondestructive testing in the building industry. In particular the major component thicknesses, the degree of reinforcement and surface coating systems make the application of NDT methods difficult. The studies first steps were undertaken to determine to which extent established applications of these techniques are useable in the field of infrastructure buildings. Methods have been evaluated that are already state of the art. So for example the ground penetrating radar was used for locating metallic mounting parts. Furthermore, the low-lying internal structure of the containment was investigated with the ultrasonic method.
The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated.
I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces.
Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PCBs, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives [1], need strong support in terms of providing them with appropriate matrix CRMs enabling the process of quality control. NMIs and DIs with proven metrological capabilities for the production and certification of such materials are necessary for the provision of quality data. This project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34 [2]. Production process includes good manufacturing practices for processing materials, method development and validation for homogeneity, stability and characterisation tests, characterisation of selected analytes together with additional information about matrix constituents, the calculation of individual uncertainties (between units inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. Inter laboratory comparison registered as EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.
Fatigue life evaluation of spar cap materials by four point bending test on width-tapered specimens
(2015)
The presented research project focuses on an effective method to evaluate the fatigue strength of thick unidirectional laminates to be applied in spar caps. Therefore, a width-tapered bending specimen was developed for a four point loading set up. Static and fatigue loading was performed with the load ratio of R=-1. The complex stress state was investigated numerically with a finite element analysis. Finally, the concept was proven experimentally on specimens made of pultruded fibre rods. The fatigue behaviour of continuous tapered width by water jet cutting was compared to discrete tapering by rod-drop.
The damage process of short glass fibre (30% weight) reinforced polyamide caused by mechanical loading was investigated from the beginning on micro cracking level to the incipient crack of mm-dimension. Based on high resolution computer tomography and the X-ray-refraction technique the inner surface due to micro-cracking at the short fibre ends and the fibre matrix debonding of the skin surface of the filament was determined quantitatively. With the knowledge of the fatigue crack propagation rate and fracture toughness of the material from former research projects, it was derived that the total inner surface due to micro cracks measured by X-ray refraction is much higher than the specimen could have withstand the load, supposed the surface is in a localized crack. Hence, the damage process could be described from micro to macro level. Accompanying fractographic investigations endorse the modelling based on the NDT-techniques.
Simulations of concrete on the mesoscale require complex geometry models that resolve single aggregates. Since they fill up to 60-80% of the virtual specimen, efficient algorithms for their placement are necessary.
Event-driven molecular dynamics (EDMD) algorithms using growing spheres are proven to create dense polydisperse sphere packings. In this paper, a modified EDMD algorithm is presented and compared to the widely used random sequential addition algorithm. It reaches denser aggregate packings and saves computation time at high volume fractions.
When meshing the geometry, a minimal distance between the aggregates ensures undistorted elements. It is obtained by increasing the aggregate size during the placement process, which makes the packing problem more challenging. For a given aggregate volume fraction, the presented algorithm maximizes this distance and meshable mesoscale geometries for concrete specimens with more than 70% aggregate content are produced.
Concrete is one of the most attractive building materials consumed by humans more than any other material, except water. The particular importance of concrete for a sustainable, energy-efficient economy is highlighted by the fact that about 5% of worldwide CO2 emissions are created from the cement industry.
Concrete is a very complex material. Its properties are time dependent, which includes the solidification after casting or creep and shrinkage. In addition, concrete is a quasi-brittle material which requires to model the softening behavior including the challenge of appropriate regularization strategies. Many characteristic features are strongly related to its complex heterogeneous structure, including particles and mortar on the mesoscale or the CSH-phases on the micro scale.
At first, a short introduction to the generation of mesoscale geometries as a three phase composite including particles, mortar matrix and the interfacial transition zone is given. Afterwards, the numerical model including meshing (XFEM and aligned meshes) as well as regularized material models for the mortar phase are presented.
The focus of the presentation is the discussion of multiscale approaches to combine mesoscale models with realistic macroscale models. This includes a concurrent approach using an adaptive transition between mesoscale and macroscale models which are coupled using the mortar method. A second hierarchical approach is based on the concept of FE², which is extended to incorporate softening by solving a fine scale boundary value problem for each macroscopic integration point.
Numerical simulation of ultrasonic wave propagation using higher order methods in space and time
(2015)
The paper discusses the efficient simulation of ultrasonic wave propagation.
It is demonstrated that a combination of higher methods in space and time leads to a significant performance boost. Higher order spectral elements are used for the spatial
discretization. A comparison with standard finite elements shows the advantages when using explicit time integration schemes. For the temporal discretization, an efficient explicit fourth order Nyström method is presented. Its computational efficiency for wave propagation problems is compared to a second order Velocity Verlet integration.
Test procedure to characterize the cracking susceptibility of RSW-steels has been developed
During externally loaded test procedure all investigated steels (HDT780CD+Z100, HDT780C+ZE75/75, HX340LAD+Z100, HCT690TD+Z100) showed a cracking behavior
With increased specimen load, the crack length grows for the micro-alloyed-steel and TRIP-steel
Complex phase steels behavior during test procedure:
Crack length growth with increasing force could not be determined
The cracking susceptibility of electro-galvanized steels is less than hot-dip galvanized steels (in this case)
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Experimental study and numerical simulation of hot crack formation for novel laser weldability test
(2015)
Hot cracking susceptibility in laser beam welding was assessed for several stainless steels by means of the CTW test
The strain rate has a significant influence on the formation of the hot crack
It was possible to determine the critical strain and strain rate that led to shot crack formation
A material ranking of hot cracking resistance could be made.A three-dimensional FEM using the contact element technique to simulate hot cracking during LBW under external load conditions was developed.
Good agreement between the strain field measured using the DIC technique and the simulation results
Susceptibility to hot cracking can be predicted by using FEM with the correct mechanical and thermo-physical material properties
Laser-GMA-hybrid welding of longitudinally welded large-diameter pipes of grades API- X80/ X120
(2015)
Potentials of the hybrid laser arc welding processes were investigated regarding reliable production of longitudinal welds of high strength pipe steels X80 and X120
Hybrid laser arc welding of the root pass:
Significant reduction in the weld cross section – savings of filler material
Lower heat input into the base material - improvement of mechanical properties of the weld joint
The arc type does not have any influence on the character of dilution in the laser part of the hybrid weld
14 mm deep root face was considered as optimum. No penetration of the filler material could be detected beyond this depth limit
Metal powder filler wires, micro alloyed with Ni and partly with Cr and Mo, guaranteed sufficient Charpy impact toughness at low temperature for the both investigated materials:
Hybrid laser arc welding is a very efficient process for the root pass in multi-pass welding and opens a large technical and economic potential for the manufacture of large pipes
As subcritical crack growth (SCCG) can reduce tensile strength of glasses by many orders of magni-tude, the potential for improvement of fatigue behaviour is most intriguing in developing ultra-strong glasses. An essential bottleneck is the basic understanding of the numerous interplaying pressure-, temperature- and water-affected relaxation phenomena at the crack tip and related toughening strat-egies. Therefore, the present project aims to advance the basic understanding of structural relaxa-tion effects and local properties caused by increased water concentration and tensile stresses at the crack tip as they are a key for structural toughening designs to develop SCCG-free glasses and glass surfaces.
Our first studies give clear evidence that glass structure and dynamics is strongly modified upon hy-dration of glasses. These changes are highly related to the nature of network formers but are affect-ed as well by the counter ions (network modifier). Results of the 1st project part suggest that struc-tural relaxation below glass transition temperature, i.e. overlapping of short-range (beta) and long-range (alpha) interactions can contribute to SCCG in water-free environments and that structurally dissolved water in the glasses can have decisive impact on this effect.
In the 2nd project stage specific glasses compositions will be investigated to gain an improved un-derstanding on the relation of sub-Tg relaxation and inert SCCG as well as to shed light to the relat-ed effects of dissolved water and its speciation. These glasses cover a broader range of different glass topologies and binding partners, whereby the coupling of alpha and beta relaxations is varied systematically by alkali-, alkaline earth ions and water species concentrations. Preparation of hy-drous glasses (up to 8 wt% water) will be performed by high pressure syntheses. Structure will be resolved by NMR, Raman and IR spectroscopy while structural relaxation is accessed in the temper-ature and frequency domain using dynamic mechanical spectroscopy and ultrasonic damping. We will focus on measurements of inert SCCG (region III) conducting experiments in vacuum and dry gas atmospheres using indentation techniques and stressing of glass specimens in DCB geometry.
Experimental data on SCCG will be provided to SPP groups, which deals with fatigue in metallic glasses and vice versa we will test theoretical predictions of ab-initio simulations of partner within SPP 1594 in order to quantify the effect of water on the crack tip. In summa topological factors con-trolling the subcritical crack growth with respect to water will be identified from which structural toughening designs for highly fatigue resistant-glasses can be derived.
Phänominilogische Studien des Blähens von bioactiven Gläsern verschiedener Zusammensetzung und Unteruschung des Einflusses einer Kristallisation. Die ausgasenden Komponenten wurden mittels Vakuumheißextraktion(VHE) und Infrarotspektroskopie identifiziert sowie der Einfluss von Korngröße, Mahldauer und -atmosphäre auf das Blähen unterucht.
Es wird der DIN-Arbeitsausschuss Ermüdungsprüfung und seine Aufgaben vorgestellt. Ferner wird über die Thematik der thermischen Drift von Extensometern und die daraus resultierenden Fehler berichtet. Darüber hinaus werden aktuelle Aspekte der dynamischen Temperaturmessung im thermo-mechanischen Ermüdungsversuch vorgestellt.
Investigations on the tensile testing procedure conducted within the European project TENSTAND
(2015)
The current presentation shows the intention of the former European TENSTAND project on computer controlled tensile testing of metals. The history of the tensile testing standards is explained. Some test results of the TENSTAND project are shown. The presentation is focused on criticism of Chinese delegates in ISO TC 164 SC1 WG4 who stated that the TENSTAND project which was finished about 10 years ago came to wrong conclusions and were misleading. This presentation points out misunderstandings of the Chinese delegation in the test program and the results of the TENSTAND project and the former development of the tensile testing standard ISO 6892-1. Some tests of the TENSTAND project were newly evaluated using the original test data. The evaluation showed again that the conclusions of the TENSTAND project are correct.
Mycotoxins are secondary metabolites of fungi which have diverse detrimental effects on humans, animals and crops. Traceable worldwide in foods and animal feeds, these contaminants cause manifold diseases and extensive economic losses. Therefore, European legislation set maximum levels of distinct mycotoxins to minimize the risks for the buying public. But standardized food analysis techniques fail to detect masked mycotoxins, whose research increasingly moves to the fore in recent years. They are formed from detoxification metabolism of plants as well as from fungi, which conjugate for example with glucosides or dihexosides. All masked mycotoxins have one thing in common: They are not detectable with standard methods, thereby contributing to the overall exposure and pose an additional health risk for the consumer.
The dissertation work will focus on the following potential new group of masked toxins. Food safety relevant mycotoxins like zearalenone and ochratoxin A possess one or more 1,3-dicarbonyl moieties. Latter are principally able to form thermodynamically stable chelate complexes with metal cations. First investigations at BAM showed interactions between zearalenone and copper ions and it is conceivable that they possibly build a complex. Our main focus is now to identify, characterize and quantify 1,3-dicarbonyl mycotoxin metal complexes as potential candidates within the group of conjugated mycotoxins.
We will simulate processes of biotransformation and identify distinct metabolites by electrochemistry coupled to liquid chromatography/mass spectrometry (EC-HPLC-MS). The obtained knowledge contributes to a better understanding of masked mycotoxins and an improved monitoring of foods and feeds, to ensure food safety.
Transport packages for spent nuclear fuel have to be assessed with respect to specific transport conditions. The physical state of the spent fuel and the fuel rod cladding as well as the geometric configuration of the fuel assemblies are important inputs for the evaluation of the package safety. The objective of this paper is to discuss the methodologies accepted by BAM for the authority assessment of spent fuel behavior within the package design approval procedure.
Tetrafluorethen wird von der Polymerindustrie seit Jahrzenten als monomeres Ausgangsmaterial sowohl für die Herstellung von Polymeren (PTFE) als auch für Kopolymere (PCTFE) eingesetzt.
Aufgrund seiner Eigenschaft als chemisch instabiles Gas kann TFE auch ohne Luftsauerstoff oder einen anderen Oxydator explosionsartig zerfallen. Nach der Initiierung des Zerfalls kann dieser unter bestimmten Bedingungen aufgrund des exothermen Reaktionsverhaltens sich selbstständig in Apparaten und Rohrleitungen ausbreiten. Dies geht aufgrund der freigesetzten Reaktionsenthalpie mit einem schlagartigen Anstieg von Druck und Temperatur einher, was zu erheblichen Belastungen der Materialien bis hin zum Versagen und Bruch und möglichen Folgeschäden einschließlich Personenschäden führen kann und in der Vergangenheit bereits mehrfach geführt hat.
Besonders nach Wartungsarbeiten besteht die Gefahr, dass Teilabschnitte im Rohrleitungssystem mit TFE, Stickstoff oder Luft gefüllt sind mit Drücken in einem Bereich zwischen technischem Vakuum und atmosphärischem Druck wohingegen angrenzende Rohrabschnitte oder Behälter immer noch TFE bei Betriebsdrücken bis 32 bar enthalten können. Dabei sind die Abschnitte in der Praxis häufig durch Kugelhähne voneinander getrennt, die aufgrund ihrer Öffnungscharakteristik bereits bei geringen Betätigungswinkeln eine große Querschnittsfreigabe für die Strömung im Rohr ermöglichen. Dadurch können schlagartige Kompressionsvorgänge des Gases im Niederdruckbereich ermöglicht werden, die allein aufgrund der thermodynamischen Zustandsänderung zu einer erheblichen Temperaturerhöhung führen und im schlimmsten Fall zur Initiierung der Zerfallsreaktion führen können.
Es wird erstmalig ein Versuchsaufbau im Industriemaßstab, der einer explosionsartigen Zerfallsreaktion von TFE standhalten kann. Zahlreiche Sicherheitskonzepte einschließlich diverser Berstscheibenkonfigurationen als auch zeitgesteuerte Schnellschlussventile wurden eingehend untersucht und bewertet, um die optimale Versuchskonfiguration für bestmögliche Reproduzierbarkeit festzulegen. Es fand eine systematische Untersuchung der schlagartigen Kompression der Systeme Luft/Luft, TFE/Luft, TFE/TFE und TFE/N2 statt.
In der Hochdrucksektion wurden Drücke bis 30 bar realisiert und im Niederdrucksektor konnten Anfangsdrücke im Bereich weniger Millibar bis hin zu Atmosphärendruck eingestellt werden.
Als Hauptergebnis wurde ein „Hazard diagram“ erstellt, mit dessen Hilfe die Zündwahrscheinlichkeit in Abhängigkeit vom Hochdruck und Niederdruck abgeschätzt werden kann. Gefährliche Bedingungen in Rohrleitungen können dadurch auf einfachem Weg identifiziert werden.
Als Referenzsystem zur Beurteilung der maximal erreichbaren nicht reaktiven Kompressions-temperaturen wurde Luft/Luft verwendet. Die damit ermittelten Daten dienten zur Bewertung von zusätzlichen exothermen Effekten, wie sie etwa bei Vorreaktion des TFE im Falle einer Dimerisierung auftreten können.
Entgegen der ursprünglichen Annahme konnten die Systeme TFE/Stickstoff und TFE/TFE im verwendeten Aufbau nicht durch Kompressionsvorgänge gezündet werden.
Die BAM erforscht mit Partnern an der TUM und DTU Methoden und Modelle für ein optimiertes Tragwerksmanagement von Infrastrukturbauwerken. Im Rahmen des vom BMVI und der BASt aufgelegten Projektclusters „Intelligente Brücke“ wurde ein Software-Prototyps zur zuverlässigkeitsbasierten Bewertung eines konkreten Spannbetonüberbaus unter Berücksichtigung von Inspektionen und Überwachungssystemen entwickelt. Der entwickelte Software-Prototyp ermöglicht Benutzern ohne vertiefte Kenntnisse der Zuverlässigkeitstheorie eine Berechnung des Einflusses von Bauwerksinformationen auf den Systemschädigungszustand und die Tragsicherheit. Auf dieser Grundlage können effiziente Inspektions- und Überwachungsmaßnahmen identifiziert und das Erhaltungsmanagement optimiert werden.
We present a concept for assessing the system reliability of monitored jacket support struc-tures of offshore wind turbines subjected to fatigue. The concept assumes that a structural health monitoring system periodically records accelerations of the jacket structure caused by ambient excitations. The recorded data is processed by a stochastic subspace-based damage detection algorithm to provide information on the global damage state of the jacket structure. This information is generally uncertain. To determine the effect of such uncertain global monitoring information on the structural reliability, the deterioration state of the jacket structure is described by a probabilistic fatigue deterioration model of all structural elements, which considers stochastic dependence among element fatigue behavior. The system deterioration model is coupled with a probabilistic structural model to compute the system failure probability. Global damage detection information is included in the reliability assessment through Bayesian updating of the system failure probability.
Introduction to PowderCell
(2015)
Die quantitative Bestimmung der Haftfestigkeit von Beschichtungen ist von entscheidender Bedeutung sowohl für die Entwicklung als auch für die Qualitätssicherung. In einer Vergleichsstudie zur Haftfestigkeit von optischen und ophthalmischen Schichten wurde mit Hilfe der Zentrifugentechnologie der Einfluss verschiedener Parameter (Substratdicke, Oberflächenvorbehand-lung, Haftvermittler) auf die Haftfestigkeit optischer Schichten auf silikatischen und ophthalmischer Schichten auf polymeren Substraten untersucht.
Zur Bestimmung der Haftfestigkeit in der physikalisch korrekten Dimension Kraft pro Fläche im Stirnabzug stehen die Ein-Proben-Prüfung mit der Zugprüfmaschine und die Mehr-Proben-Prüfung mittels Zentri- fugentechnologie zur Verfügung. Die Zentrifugentechnologie wurde ausgewählt, da die Prüfung von bis zu acht Proben unter nahezu identischen Versuchsbedingungen und somit eine statistisch gesicherte Bestimmung der Haftfestigkeit möglich sind.
Es konnte nachgewiesen werden, dass die Substratdicke einen erheblichen Einfluss auf die gemessene Haftfestigkeit hat. Dies entspricht den Erwartungen, da es sich bei der Haftfestigkeit um eine System- eigenschaft des Schicht-Substrat-Systems handelt. Bei den Delaminationsbrüchen (DF) konnte zwischen Delamination des metallischen Reflektors (DF-R) und Delamination des Dielektrikums (DF-D) unter- schieden werden. Im Fall hinreichender Haftfestigkeit der Beschichtung traten auch Adhäsionsbrüche am Interface zum und Kohäsionsbrüche im Klebstoff auf. Nachfolgende Untersuchungen werden sich mit alternativen Klebstoffen und weiterentwickelten Fügestrategien befassen.
The design of sample flow cells, commonly used in online analytics and especially for medium resolution NMR spectroscopy (MR-NMR) in low magnetic fields, was experimentally and theoretically investigated by 1H-NMR and numerical simulations. The flow pattern was characterised to gain information about the residence time distribution and mixing effects. Both 1H-NMR imaging and spectroscopy were used to determine the characteristics of flow cells and their significance for on-line measurements such as reaction monitoring or hyphenated separation spectroscopy. The volume flow rates investigated were in the range from 0.1 to 10 ml/min, typically applied in the above mentioned applications. When compared to those commonly used in high-field NMR, the special characteristics of flow cells for MR-NMR were revealed by various NMR experiments and compared with CFD simulations. The influence of the design of the inlet and outlet on the flow pattern was investigated as well as the effect of the length of the cell. For practical use, a numerical estimation of the inflow length was given. In addition, it was shown how experiments on the polarisation build-up revealed insight into the flow characteristics in MR-NMR.
Properties and application areas of photon counting and energy resolving digital detector arrays
(2015)
Since a few years the direct detection of X-ray photons into electrical signals is allowed by usage of highly absorbing photo conducting materials (e.g. CdTe) as detection layer of an underlying CMOS semiconductor X-ray detector. NDT energies up to 400 keV are today also possible. The image sharpness and absorption efficiency is improved by the replacement of the unsharp scintillation layer (as used at indirect detectors) with a photo conducting layer of much higher thickness and a high voltage across it. If the read-out speed is high enough (ca. 50 – 100 ns dead time) single X-ray photons can be counted and their energy measured. Read-out noise and dark image correction can be avoided. By definition of energy thresholds selected energy ranges of the X-ray spectrum can be detected or also suppressed. This allows material discrimination by dual-energy technique or the reduction of image contributions from scattered radiation, which results in an enhanced contrast sensitivity. To use these advantages in an effective way, a special calibration procedure has to be developed, which considers also time dependent processes in the detection layer. This contribution presents some of these new properties of direct converting DDAs in comparison to the conventional indirect converting detectors for fiber composites and thick walled steel pipes (up to 35 mm wall thickness). Possible new application areas of NDT will be discussed for material discrimination especially within fiber reinforced composites (e.g. CFRC und GFRC).
Die Verleihung des Deutschen Zukunftspreises an ein Team zum Thema "Ultrakurzpulslaser für die industrielle Massenfertigung - Produzieren mit Lichtblitzen" im Jahr 2013 belegt die industrielle Relevanz des Ultrakurzpulslasereinsatzes in der Materialbearbeitung. Zunehmend werden weitere Anwendungen z.B. in der Mess- und Medizintechnik erschlossen. Femtosekunden-Laserpulse weisen prinzipbedingt ein breites Spektrum auf und besitzen bereits bei moderaten Pulsenergien extreme Pulsspitzenleistungen, womit über „konventionelle“ Laserquellen hinausgehende Herausforderungen an den Laserschutz entstehen. Die in entsprechenden Laserschutzbrillen verwendeten Laserschutzfilter müssen eine große spektrale Absorptionsbandbreite aufweisen und dürfen nicht aufschalten, d.h. keine induzierte Transmission zeigen. Im Vortrag soll dargestellt werden, dass Laserschutzfilter auf Glasbasis, die über ein breites Absorptionsspektrum verfügen, einen ausreichenden Schutz gegenüber fs-Laserstrahlung bieten, wohingegen Laserschutzfilter auf Polymerbasis eine induzierte spektrale Transmission bei steigender Energiedichte aufweisen können, was zu einem drastischen Verlust der Schutzfunktion führt.
Due to recent advances in technical developments of NMR instruments such as acquisition electronics and probe design, detection limits of components in liquid mixtures were improved into the lower ppm range (approx. 5–10 ppm amount of substance). This showed that modern NMR equipment is also suitable for the observation of hydrocarbon samples in the expanded fluid phase or gas phase. Since Quantitative NMR spectroscopy (qNMR) is a direct ratio method of analysis without the need of calibration it was used to determine impurities in appropriate liquid and liquefied hydrocarbon isomers up to C6, which are used for preparation of primary gas standards, e.g., natural gas or exhaust gas standards. At the same time it is possible to yield structural information with a minimum of sample preparation. Thus, cross contaminations between different isomers of the observed hydrocarbons and their (NMR-active) impurities can be identified and quantified.
In general, most quantitative organic chemical measurements rely on the availability of highly purified compounds to act as calibration standards. The traceability and providence of these standards is an essential component of any measurement uncertainty budget and provides the final link of the result to the units of measurement, ideally the SI. The more recent increase in the use of qNMR for the direct assessment of chemical purity however can potentially improve the traceability and reduce the uncertainty of the measured chemical purity at a reduced cost and with less material. For example the method has beneficially been used by National Measurement institutes for recent CCQM comparisons including the CCQM–K55 series of purity studies.
Traditional ‘indirect’ methods of purity analysis require that all impurities are identified and quantified, leading to a minimum of 4 individual analytical methods (organic impurities, water, solvents, inorganic residue). These multiple technique approaches measure an array of different chemical impurities normally present in purified organic chemical compounds. As many analytical methodologies have compound-specific response factors, the accuracy and traceability of the purity assessment is dependent on the availability of reference materials of the impurities being available.
qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The development of CRMs addressing qNMR specific measurement issues will give analysts compounds ideally suited for the analytical method and also provide full characterisation of qNMR related parameters to enable more realistic uncertainty budgets. These materials will give users the tools to exploit qNMR more easily and enable them to speed up analytical method development and reduce the time and financial burden of multiple analytical testing.