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Die Kenntnis von Materialeigenschaften spielt bei der Entwicklung oder Optimierung von Betonen und Bauweisen für den Straßenbau sowie der Qualitätssicherung eine bedeutende Rolle. Gleichermaßen bilden physikalische Materialkennwerte die Grundlage für die rechnerische Dimensionierung und die Restsubstanzbewertung von Betonfahrbahndecken. Eine relevante Kenngröße bei der Untersuchung thermisch induzierter Spannungs- und Verformungszustände stellt der thermische Ausdehnungskoeffizient dar. Im Zuge der systematischen Weiterentwicklung der rechnerischen Dimensionierung, aber auch im Zusammenhang mit der gezielten Verbesserung der Gebrauchseigenschaften von Betonfahrbahndecken gilt es zu hinterfragen, ob lastunabhängige Formänderungseigenschaften der verwendeten Betone aktuell ausreichend Beachtung finden, ob allgemeine Literaturwerte für die heutigen Fahrbandeckenbetone stets Gültigkeit besitzen und ob deren Implementierung in numerische Modelle zu realitätsnahen Vorhersagen führt. Für eine empirische Herangehensweise ist die Verfügbarkeit adäquater Prüfverfahren von entscheidender Bedeutung. In Deutschland existiert aktuell jedoch kein standardisiertes oder genormtes Verfahren für die prüftechnische Bestimmung des thermischen Ausdehnungskoeffizienten von Beton. Daher wurden unter Beachtung straßenbauspezifischer Gesichtspunkte zwei Prüfansätze entwickelt, die in diesem Beitrag vorgestellt sowie hinsichtlich möglicher Messunsicherheiten und Messungenauigkeiten diskutiert werden. Außerdem werden ausgewählte Ergebnisse aus Analysen an Bestandsbetonen aus dem BAB-Netz dargestellt. Im Ergebnis sollen die Untersuchungen einen Beitrag zur Schaffung der prüftechnischen Voraussetzungen für eine abgesicherte Quantifzierung der thermischen Dehnung von Fahrbahndeckenbetonen leisten.
Die additive Verarbeitung hochfester Feinkornbaustähle mittels Wire Arc Additive Manufacturing (WAAM) ist ein komplexes, aber zugleich auch effizientes Verfahren, bei dem Werkstoff, Bauteilgeometrie und Schweißprozess gezielt aufeinander abgestimmt sein müssen. Ziel dieser Studie war es, einen Zusammenhang zwischen den Prozessparametern und der generierten Schichtgeometrie zu ermitteln. Dazu wurden definierte Referenzkörper mit einem robotergestützten Schweißsystem additiv gefertigt und hinsichtlich Schichthöhe, Wandstärke und Mikrostruktur analysiert. Fokus der Untersuchung waren sowohl konventionelle als auch für die WAAM-Fertigung speziell entwickelte hochfeste Schweißzusatzwerkstoffe. Die geometrischen Eigenschaften additiv gefertigter Bauteile lassen sich insbesondere durch die Faktoren Drahtvorschubgeschwindigkeit und Schweißgeschwindigkeit gezielt einstellen. Jedoch können diese Parameter nicht beliebig variiert werden, auch aufgrund der rheologischen Eigenschaften der Zusatzwerkstoffe. Zu hohe Streckenenergien führen zu lokalen Überhitzungen und Fehlstellen in der generierten Schicht. Undefinierte Fließ- und Erstarrungsvorgänge im überhitzten Bereich erschweren die maßhaltige Fertigung. Deshalb wird bei speziellen WAAM-Schweißdrähten das Fließverhalten gezielt modifiziert, sodass es über einen größeren Temperaturbereich hinweg konstant ist. Erst die Kenntnis über die komplexen Zusammenhänge zwischen den Prozessparametern und der Bauteilgeometrie ermöglicht die Erzeugung exakter Schichtmodelle für die additive Fertigung. Dies bildet die Grundlage für die Bearbeitung weiterer Fragestellungen auf dem Gebiet der additiven Fertigung mit hochfesten Zusatzwerkstoffen und insbesondere deren Anwendung in modernen hochfesten Bauteilen.
In 2019 over 30 000 people were killed or injured by explosions caused by explosives like TNT, PETN, HMX and RDX. Therefore, highly sensitive assays for the detection of TNT are needed. In this study we compared two commercially available TNT antibodies: A1.1.1 and EW75C with a highly optimized indirect competitive ELISA based on a BSA-TNA conjugate. As a result, a precision profile for both antibodies was determined with a LOD of 170 pmol L-1 for the clone A1.1.1 and a LOD of 3,2 nmol L-1 for the clone EW75C. The measurements showed that the clone A1.1.1 is a highly sensitive antibody for the detection of TNT while the clone EW75C does show medium performance at most.
In the cross-reactivity characterization of both antibodies many substances, closely related to the structure of TNT were tested. Both antibodies showed strong cross reactivity with trinitroaniline and trinitrobenzene. For the clone A1.1.1, which is known to originate from immunization of mice with an TNP-glycine-KLH conjugate, this has to be expected. Interestingly the clone EW75C, which was not characterized yet, showed similar behavior. This suggests a TNA-conjugate as immunogen for the EW75C antibody as well. None of both antibodies showed cross-reactions to the high explosives PETN, HMX and RDX. Also, the cross-reactions of nitro musks with the antibodies were investigated. Despite their prohibition, nitro musks are still used in Asia especially and are particularly popular in India. The overall superior clone A1.1.1 showed a significant cross-reactivity to musk ambrette. For practical reasons the influence of musk ambrette on this assay when used in natural environment should be investigated.
In further experiments, the highly sensitive TNT antibody A1.1.1 was digested with papain to obtain monovalent Fab-fragments. Due to its high stability against the digestion, a custom protocol for the IgG1 subclass of mice, to which the clone A1.1.1 belongs, was developed, resulting in a quantitative digestion of the intact antibody to Fab fragments. The success of the digestion was determined with MALDI-TOF-MS and SDS-PAGE. It was shown that this protocol worked for many different antibodies of IgG1 subclass as well.
Es wurde im Rahmen dieser Arbeit eine neue Methode der Biokonjugation entwickelt, die es ermöglicht humane Antikörper ortspezifisch mit IgG-bindenden Peptiden zu konjugieren. Als Basis fungierte ein Peptid, welches für den Einsatz gezielt modifiziert wurde. So sollte am C-Terminus ein Biotin eingefügt werden, dass für die spätere Detektion der Biokonjugation genutzt werden kann, während am N-Terminus ein Cross-Linker für die kovalente Bindung zum Antikörper eingefügt wurde. Das Biotin wurde mittels Biotin-Lysin eingebaut. Dies hat den Vorteil, dass die modifizierte Aminosäure direkt in der SPPS genutzt werden kann. Auch der Cross-Linker soll schon während der SPPS in das Peptid integriert werden. Als Cross Linker wurden die zwei heterobifunktionellen Succinimidyl(3-bromoacetamid)propionate und Succinimidyl(4-iodacetyl)aminobenzoat untersucht. Die Aktivierung des Peptides mit dem SBAP-Cross-Linker erfolgte am besten im pH-Bereich zwischen 7,0 und 9,0. Die Modifizierung des Peptides mit dem Iodid-Cross-Linker SIAB unter den gleichen Bedingungen zeigte allerdings keine zufriedenstellenden Ergebnisse. Da das erste Peptid allerdings in den Folgeexperimenten sehr gute Ergebnisse zeigte, musste kein weiterer Linker getestet werden. Zusätzlich zu der Cross-Linker-Wahl sollte der Abstand zwischen dem Cross-Linker und dem Grundgerüst des Peptides auf den Einfluss der Bindung untersucht werden. Dazu wurden drei Kontrollpeptide synthetisiert, die entweder um zwei Aminosäuren zwischen dem ursprünglichen N-Terminus des Peptides und dem SBAP-Linker verlängert wurden, keinen SBAP-Linker beinhalten oder die Verlängerung ohne SBAP-Linker besaßen. Die erfolgreiche Synthese aller vier Peptide wurde mittels MALDI-TOF-MS bestätigt.
Sulfate is abundant in the environment and, as a result, sulfate-containing minerals constitute a large and important focus of research. These minerals play an important role in many geochemical and industrial processes, including the sulfur cycle, the construction industry (e.g., plaster of Paris), fault tectonics, acid mine drainage, and even rare biominerals. Important to note are the abundant amounts of sulfate (minerals) located on the surface of Mars, and in meteorites, extending the relevance of this mineral group beyond the realm of our planet. In geological systems, sulfate minerals such as barite are also important for indicating certain sedimentation environments. In this regard, sulfate deposits can be used to evaluate the redox state of ancient oceans during early Earth time periods.
CHG is very different compared to other graphite degenerations or defects;
Filigree, multi-branched string-like, 3d interconnected structure;
Morphology and volumetric amount of CHG cannot be accessed by stereological interpretation of 2d section data;
Field-tested, technically established method to quantify CHG in components not available;
Fatigue: CHG causes substantial reduction in fatigue limit and significant increase in crack growth rate;
Therefore: Avoid or exclude CHG!
High-entropy alloys containing up to 6 platinum group metals can be prepared by thermal decomposition of single-source precursors non requiring high temperature. We prepare the first example of a single-phase hexagonal high-entropy alloy. Heat treat- ment up to 1500 K and compression up to 45 GPa do not result in phase changes, a record temperature and pres- sure stability for a single-phase high-entropy alloy. The alloys show pronounced electrocatalytic activity in methanol oxidation, which opens a route for the use of high-entropy alloys as materials for sustainable energy conversion.
The Scythica Vindobonensia, the new fragments on Gothic incursions into Roman provinces in the Balkans in the middle of the third century AD that were revealed some years ago in a Greek palimpsest at the Austrian National Library in Vienna (ÖNB), are commonly considered as one of the most important additions of the last decades to the corpus of texts from classical Antiquity. Tere is a high degree of confdence among scholars in supposing that the fragments come from the lost work Scythica written in Greek by the third-century historian P. Herennius Dexippus (Δέξιππος) of Athens. The new fragments have hence also been called Dexippus Vindobonensis. In his Scythica, Dexippus recorded wars of the Romans with the Goths (and other tribes) whom he called Scythians.
The work had been hitherto known only from excerpts and quotes by later authors. Eight pages of a Byzantine manuscript copy of the ancient text have survived hidden underneath the visible surface of the last four parchment folios of the Vienna manuscript Historicus graecus 73, f. 192r -195v4. The copy is written in a Greek calligraphic minuscule which has been estimated by palaeographers to be of the middle or the second half of the eleventh century. In the thirteenth century, the text (on each of the eight pages arranged in one column, with 30 lines per page) was washed of the parchment and the valuable material made from animal skin was re-used for Christian texts. The new writing largely covered the faded remnants of the original text. It thus became hidden from the human eye for more than seven hundred years. Its discovery by Jana Grusková, a classical philologist specialized in the transmission of Greek texts, resulted from a systematic review of all Greek palimpsests kept at the Austrian National Library in Vienna at the beginning of the twenty-first century and a detailed examination of the four folios in 2007-20097.
High and medium entropy alloys gained increasing academic and industrial interest as novel materials for engineering applications. This project is aiming to clarify and compare the general and local corrosion properties of high entropy alloy CrMnFeCoNi and medium entropy alloy CrCoNi in different aqueous environments. The focus lies on the local corrosion processes that result either from microstructural imperfections (inclusions, defects at grain boundaries etc.) in the base material or processing related changes in the microstructure and/or local composition.
The corrosion behavior of the alloys was monitored via potentiodynamic polarization experiments and the local corrosion characteristics were further investigated by means of scanning electrochemical microscopy (SECM). Their passivation behavior was analyzed in three different electrolyte systems (NaCl, H2SO4 and NaClO4; c = 0.1M). The characterization of the surface morphology and composition of the passive film was performed by means of atomic force microscopy (AFM), scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy (SEM/EDX) and X-Ray photoelectron spectroscopy (XPS), respectively.
Considering long term corrosion effects, electrochemical work was supported with immersion tests and the analysis of corrosion products by SEM/EDX and XPS depth-profiling. Our results indicate that the medium entropy alloy CrCoNi has a significantly higher corrosion resistance in comparison to the high entropy alloy CrMnFeCoNi. The presentation will summarize some of our results on the mechanistical aspects of the observed high corrosion resistance.
Within the scope of this work, a laser implantation process has been used, in order to improve the tribological performance of hot stamping tools. This surface engineering Technology enables the generation of dome-shaped, elevated and highly wear resistant microfeatures on tool surfaces in consequence of a localized dispersing of hard ceramic particles via pulsed laser radiation.
As a result, the topography and material properties of the tool and thus the tribological interactions at the blank-die interface are locally influenced. However, a suitable selection of hard ceramic particles is imperative for generating defect-free surface features with a high share of homogenously disturbed particles. For this purpose, different niobium (NbB2 and NbC) as well as titanium-based (TiB2 and TiC) materials were embedded on hot working tool specimens and subsequently analyzed with regard to their resulting shape and mechanical properties. Afterwards, modified pin-on-disk tests were carried out by using conventional and laser-implanted tool surfaces, in order to evaluate the wear and friction behavior of both tooling systems.
In der Automobilindustrie stellt das Presshärteverfahren eine Schlüsseltechnologie zur ressourceneffizienten Herstellung sicherheitsrelevanter Karosserie-komponenten dar. Während der Umformoperation treten jedoch hohe Reibungs- und Verschleißerscheinungen an den interagierenden Werkzeug- und Werkstückwirkflächen auf, die sowohl die Bauteilqualität als auch die Maschinenstandzeit nachhaltig beeinträchtigen. Um die bestehenden Verfahrensgrenzen zu erweitern, wird daher eine Modifikation der Presshärtewerkzeuge mittels Laserimplantation angestrebt. Hierbei werden in die Werkzeugoberfläche keramische Hartstoffpartikel anhand eines gepulsten Laserstrahles eingebettet, infolgedessen kuppelförmige sowie höchstfeste Strukturen im Mikrometerbereich entstehen. Die Auswahl geeigneter Hartstoffmaterialien stellt jedoch ein entscheidendes und bisweilen limitierendes Kriterium dar, um defektfreie sowie verschleißresistente Oberflächenmodifikationen zu generieren. In diesem Zusammenhang wurden im Rahmen dieser Arbeit unterschiedliche titanbasierte Hartstoffpartikel auf presshärtespezifische Werkzeugstähle laserimplantiert und anschließend mittels modifizierten Pin-on-Disk-Tests hinsichtlich ihres tribologischen Einsatzverhaltens untersucht. Um die Wirksamkeit des Laserimplantationsverfahrens zu evaluieren, wurden zudem Verschleißuntersuchungen an unmodifizierten Werkzeugoberflächen durchgeführt und mit den erzielten Ergebnissen der lokal dispergierten Topographien verglichen.
The fracture mechanics-based IBESS approach is applied to the determination of FAT classes of butt welds with crack Initiation along the weld toe. The aim is an investigation of the effect of the geometrical parameters toe radius, flank angle, reinforcement and secondary notches such as roughness or undercuts. The influence of these parameters is discussed both individually and in combination; however, excluding statistical distributions of them and the material data. The results, when compared with conventional FAT classes for butt welds, are encouraging with respect to a potential contribution of IBESS to the discussion of more advanced quality criteria for welds. To that purpose, demands for further research are proposed.
While there is a permanent improvement of concrete pavement mixtures and pavement construction types over the last decades, the state-of-the-art joint sealing materials and joint constructions seem to stagnate on an antiquated empirical level. This status has been reaffirmed in the latest European standard. The consequences in the motorway network due to unsatisfying capability and durabilty of joint sealing systems are unacceptable. In addition, inadequate traffic performance (noise emissions, roll-over comfort) and traffic safety losses in the joint area of concrete pavements are existing challenges. These deficits and weaknesses reflect a demand for joint sealing materials and constructions whose approval requirements take functional aspects into account. Furthermore a sufficient analysis of decisive loads and a practice-oriented method to evaluate the requirements towards performance and durability is still missed. In this contribution decisive loads to German highways are analyzed. The design of test specimen for representative functional testing of joint sealing systems is discussed. The focus is on the geometry of the test specimens and the used concrete mixture. Finally, a new approach for a function-orientated test concept that considers representative load functions is presented. The potential of this approach to validate the durability and capability of various joint sealing systems is also presented using an example.
Die Bemessung von tragendem Lehmmauerwerk erfolgt in Deutschland auf Basis der Lehmbau Regeln. Das dort verankerte Nachweisverfahren beruht auf einem globalen Sicherheitskonzept, welches aus zuverlässigkeitstheoretischer Sicht nicht mehr dem Stand der Technik entspricht. Auf Grund dessen wird das Bemessungskonzept für Lehmmauerwerk vom Deutschen Institut für Bautechnik (DIBt) voraussichtlich 2023 außer Kraft gesetzt. Ein statischer Nachweis von tragenden Lehmbauten wäre in Deutschland dann ausschließlich mit einer Zustimmung im Einzelfall (ZiE) oder vorhabenbezogener Bauartgenehmigung (vBg) möglich. Beides ist mit erheblichem Mehraufwand und höheren Kosten verbunden, was für den Lehmmauerwerksbau einen entscheidenden Nachteil im Vergleich zum konventionellen Mauerwerksbau darstellt. Um eine unkomplizierte Praxisanwendung von Lehmmauerwerk zu ermöglichen, werden innerhalb eines Forschungsvorhabens, welches von der Bundesanstalt für Materialforschung und -prüfung (BAM), dem Institut für Massivbau der Technischen Universität Darmstadt sowie dem Ingenieurbüro ZRS durchgeführt wird, auf Basis der Produktnormen für Lehmsteine und Lehmmauermörtel Grundlagen für ein aktualisiertes Bemessungskonzept entwickelt. Im Rahmen des Projekts wird ebenfalls untersucht, inwiefern die Bemessungsregeln nach den vereinfachten Berechnungsmethoden für unbewehrtes Mauerwerk gemäß DIN EN 1996-3 / NA auf den Lehmmauerwerksbau übertragbar sind. Falls eine Anwendung des normativen Nachweisverfahrens bei Lehmmauerwerk möglich ist, wäre zukünftig eine Aufnahme von Lehmsteinen und Lehmmauermörtel in den nationalen Anhang des Eurocode 6 denkbar, was eine bedeutsame Erweiterung des Anwendungsbereichs von Lehmmauerwerk zur Folge hätte.
Diverse wissenschaftliche Untersuchungen konnten zeigen, dass bemessungsrelevante Festigkeits- und Verformungseigenschaften von Lehmmauerwerksbaustoffen stark von der vorherrschenden Materialfeuchte abhängen, welche im hygroskopischen Wassergehaltsbereich im Wesentlichen von der relativen Luftfeuchte (RLF) bestimmt wird. Auch die Zwischenergebnisse des laufenden Forschungsvorhabens zur Entwicklung eines Bemessungskonzepts für Lehmmauerwerk ergaben eine deutlich erkennbare Abhängigkeit zwischen der Materialfeuchte und den relevanten Festigkeits- und Verformungseigenschaften. Eine detaillierte Kenntnis des feuchteabhängigen Materialverhaltens von Lehmsteinen, -mörtel und -mauerwerk ist zwingend erforderlich, um ein konsistentes und zuverlässiges Bemessungskonzept für Lehmmauerwerk zu entwickeln. Im Rahmen des laufenden Forschungsprojektes werden deshalb umfangreiche Versuche zum Drucktragverhalten von Lehmsteinen und -mörtel sowie Lehmmauerwerk nach Konditionierung bei unterschiedlichen RLF durchgeführt und analysiert. Weiterhin werden auf Basis der experimentellen Ergebnisse numerische Modelle kalibriert, welche die detaillierte Analyse der Biegedrucktragfähigkeit von Lehmmauerwerk ermöglichen.
In diesem Beitrag werden zunächst die bisherigen Zwischenergebnisse bezüglich der experimentell ermittelten feuchteabhängigen Materialkennwerte von Lehmsteinen, -mörtel und -mauerwerk dargelegt. Darauf aufbauend werden numerische Untersuchungen zur Bestimmung der Systemtragfähigkeit von Lehmmauerwerk unter Feuchteeinflusses durchgeführt und erläutert.
Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements
(2020)
In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles.
The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum.
1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties.
2. Iron oxide nanoparticles are under development as new candidate reference material at BAM.
3. Narrow particle size distribution confirmed by light scattering and electron microscopy.
Für die Bestimmung der Restlebensdauer zyklisch beanspruchter Bauteile kommt dem Schwellenwert für Ermüdungsrissausbreitung ∆Kth und dem sich anschließenden Schwellenwertbereich der da/dN-∆K-Kurve große Bedeutung zu. Dem stehen Unsicherheiten bei der Bestimmung und Analyse gegenüber. Der Aufsatz befasst sich mit der Ermittlung des sogenannten intrinsischen Schwellenwerts, der als robuster Eingangsparameter für eine „rissschließfreie“ Analyse der Restlebensdauer von entscheidender Bedeutung ist.
The longitudinal and transverse strength of three unidirectional thermoplastic prepreg systems: carbon fiber/polypropylene (CF/PP), polyamide 6 (CF/PA6), and polyphenylene sulfide (CF/PPS) are studied and analytical formulas are proposed for the estimation of matrix and fiber/matrix interface properties from composites properties. Since the matrices are semi-crystalline thermoplastics, the influence of cooling rate on the strength is statistically evaluated. While the 0° tensile strength is found to be independent of the cooling rate, the 90° tensile strength is strongly influenced by the matrix type and cooling rate. The matrix modulus increases as the cooling rate is decreased; the degree of crystallinity also increases. The matrix residual stress, interfacial shear strength, and mode II interlaminar fracture toughness are also found to depend on the cooling rate, with the trends different for different matrices.
In the face of rising energy demand and the impending climate change the development of a sustainable, fossil-free fuel and chemical production is of global importance. One possible goal is the development of electrochemical conversion processes using catalysts. Porous materials play an important role in such energy applications. The key to the development of improved catalysts is a better understanding of the relations between their performance, stability and physico-chemical properties. However, the complex morphology of such catalysts constitutes a challenge even for modern analytical techniques.
Spectroscopic ellipsometry (SE) is a versatile method for studying material properties by using appropriate models (e.g. film thickness, optical and electronic properties). The fact that the material properties cannot be taken directly from the measured spectra, the developed models have to be validated. In a first step, the model for the ellipsometric fit studies of a calcination series of mesoporous iridium oxide films (300 – 600 °C) was investigated and validated with respect to their material properties. Moreover, the electronic structures of the catalysts reveal a direct correlation with electrochemical activities. The development of an environmental cell offers the possibility of investigations under real conditions. This will allow changes in the optical and electronic properties during the electrocatalytic oxygen evolution reaction.
Die Verwendung von LTT-Zusatzwerkstoffen stellt einen alternativen Ansatz zu den sonst üblichen Verfahren der Schweißnahtnachbehandlung zur Schwingfestigkeitserhöhung geschweißter Stahlkonstruktionen dar. Der wesentliche Wirkmechanismus beruht auf der Beeinflussung des Eigenspannungszustands durch die niedrige Martensitstarttemperatur bereits während des Schweißens. Dadurch werden die Druckeigenspannungen aus der behinderten Volumenausdehnung infolge Phasenumwandlung voll wirksam. Weiter weist die Schweißnaht eine hohe Härte auf, die die Schwingrissbildung verzögern kann, allerdings auch zu einer niedrigen Kerbschlagarbeit führt.
Im vorliegenden Forschungsvorhaben wurden grundlegende Untersuchungen zur schweißtechnischen Verarbeitung eines LTT-Zusatzwerkstoffes durchgeführt. Dies beinhaltet die Sicherstellung der Schweißbarkeit sowie die Charakterisierung der Verbindungseigenschaften.
Untersuchungen zur Schweißeignung machten deutlich, dass ein sicherer Einsatz in dem für hochfeste Stähle zur Verfügung stehenden Arbeitsfenster möglich ist. Der verwendete LTT-Zusatz auf Cr-Ni-Basis lässt sich mit hoher Nahtgüte fügen. Auch die mechanischen Eigenschaften erlauben den Einsatz im Bereich hochfester Stähle mit einer Streckgrenze von 960 MPa. Entwicklungspotential gibt es hinsichtlich der Zähigkeit. Die in dieser Arbeit erreichten Kerbschlagwerte liegen deutlich unter denen kommerziell verfügbarer konventioneller Schweißgüter. Die Untersuchungen belegen, dass der Effekt der martensitischen Phasenumwandlung im gesamten Schweißgut zum Tragen kommt. Die angestrebten hohen Druckeigenspannungen finden sich vornehmlich im Schweißgutinnern.
Im weiteren Vorgehen wurden Schwingfestigkeitsuntersuchungen an den Stählen S355J2 und S960Q unter Verwendung konventioneller Zusatzwerkstoffe im Vergleich zum LTT-Zusatz durchgeführt. Die verwendeten Konstruktionsdetails sind ein Stumpfstoß unter Variation der Schweißnahtausführung (DY-Naht und V-Naht), ein Kreuzstoß mit HV-Naht sowie ein Überlappstoß mit einseitig und beidseitig geschweißter Kehlnaht.
Weitergehend wurde eine bauteilähnliche Probe (die Längssteife) untersucht, bei der der LTT-Zusatzwerkstoff als zusätzliche Schweißlage aufgebracht wurde. Neben der Schwingfestigkeit wurden die Schweißnähte hinsichtlich der Eigenspannungen, der Eigenspannungsstabilität im Schwingversuch sowie metallografisch charakterisiert.
Eine generell positive Wirkung des LTT-Zusatzwerkstoffes im Hinblick auf die Schwingfestigkeitssteigerung kann nicht bestätigt werden. Teilweise ist eine Steigerung der Schwingfestigkeit bei Substitution konventioneller Zusatzwerkstoffe zu beobachten, teilweise zeigt sich kein Effekt. Ursächlich hierfür ist die bei manchen Stoßformen mangelnde Steifigkeit quer zur Schweißnaht, die zur Ausbildung hoher Druckeigenspannungen infolge Phasenumwandlung notwendig wäre. Die bauteilähnliche Längssteife bestätigt allerdings das grundlegende Potential der LTT-Zusatzwerkstoffe bei Vorliegen hinreichender Steifigkeit.
High power laser beam welding has been already introduced in ship building industry since last two decades and is characterized by higher performance as conventional arc welding technologies through its higher welding speed, penetration depth and therefore higher productivity. Moreover, high quality weld joints are achievable thanks to a stronger automatization degree and better repeatability of the process. A further advantage of the laser beam welding is a manufacturing of parts with very low distortion according to much lower heat input, so that rework amount can be reduced significantly. Nevertheless, there are still some unresolved problems limiting the range of application of the technology in part manufacturing within ship building industry, restricted by development and application of new materials or new design of ship vessels.
The present contribution deals with some novel aspects of laser beam welding technology allowing to widen this range significantly. One of the possibilities is to increase the weld seam thickness for single pass laser or laser-hybrid welding is to apply contactless EM-support system based on generation of the Lorentz force counteracting the liquid metal drop out. Also, application of laser-hybrid welding technology for welding novel materials like cold resistant steel X8Ni9 used for construction of LNG tanks brings technological and design advantages comparing to conventional welding technologies by using of a similar alloyed filler wire instead of expensive Ni-based filler material. Finally, it is shown how the application of computational techniques can be used to helps to improve the quality of laser welded joints and avoid the critical weld failure by optimization of the welding process parameters.
Modern air-liners and rotor blades of wind turbines are basically made of fiber reinforced plastics (FRP). Their failure heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report on in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics (CFRP) due to inter fiber failure. An in-house designed compact-tensile testing machine with a load range up to 15 kN was integrated into the beam path. Since conventional radiographs do not reveal sufficient contrast to distinct cracks due to inter fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging technique (DEI) is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. In the laboratory, scanning X-ray refraction topography of CFRP has been applied long before but it comes along with several disadvantages: the long total measuring time hampers real time (in-situ) measurements and the required small beam size hinders end-to-end imaging. The introduced technique overcomes both drawbacks. Imaging and tensile test rig are run unsynchronized at the greatest possible frame rate (0.7 s-1 at 28.8 µm pixel size) and smallest possible strain rate (5.5∙10-4 s-1). For 0°/90° non-crimped fabrics (ncf) the first inter fiber cracks occurred at 380 MPa (strain 0.7 %). Prior to failure at about 760 MPa (strain 2.0 %) we observe the evolution of a nearly equidistant 1 mm grid of cracks running across the entire sample in the fully damaged state before total failure.
Insight of the thermal decomposition of ammonium hexahalogenoiridates(IV) and hexachloroiridate(III)
(2020)
Thermal decomposition of (NH4)3[IrCl6]·H2O, (NH4)2[IrCl6] and (NH4)2[IrBr6] in reductive and inert atmospheres has been investigated in situ using quick-EXAFS and temperature-resolved powder X-ray diffraction. For the first time, (NH4)2[Ir(NH3)Cl5] and (NH4)2[Ir(NH3)Br5] have been proven as intermediates of thermal decomposition of (NH4)3[IrCl6]·H2O, (NH4)2[IrCl6] and (NH4)2[IrBr6]. Thermal degradation of (NH4)2[IrCl6] and (NH4)2[IrBr6] is a more complex process as suggested previously and includes simultaneous formation of (NH4)2[Ir(NH3)Cl5] and (NH4)2[Ir(NH3)Br5] intermediates mixed with metallic iridium. In the inert atmosphere, complexes (NH4)[Ir(NH3)2Cl4] and (NH4)[Ir(NH3)2Br4] as well as [Ir(NH3)3Br3] were proposed as possible intermediates before formation of metallic iridium particles
Notch impact toughness of laser beam welded thick sheets of cryogenic nickel alloyed steel X8Ni9
(2020)
The paper deals with the investigations of the impact toughness of laser beam welded 14.5 mm thick sheets made of cryogenic steel X8Ni9 as a function of preheating. This 9% nickel alloyed steel is widely used in the liquefied natural gas (LNG) industry. An application of highly efficient welding processes such as high-power laser beam welding (LBW) in LNG sector requires an understanding of the interactions between the LBW process parameters and weld properties, in particular the impact toughness. The results show that the original fine-grained martensitic microstructure of the base metal (BM) is significantly changed by melting and crystallization during the LBW, what can lead to a decrease in the impact toughness of the weld metal (WM) below the required level. An optimal preheating temperature range leads to the favorable thermal welding cycle and is of remarkable importance for maintaining the notch impact toughness of laser beam welded joints of these thick steel sheets. A parameter window was identified in which V-notch impact toughness comparable to that of the BM at -196 °C was achieved.
The study deals with the application of the high-power hybrid-laser arc welding process on up to 15 mm thick pipe segments with the intention to avoid end crater imperfections during closing of the circumferential welds, where the pipes were turned during welding in 1G- and 2Gpositions.
Different techniques such as laser power ramp-down, abrupt switch-off of the laser power and change of the magnification of the laser spot diameter and defocusing of the laser beam relative to the workpiece were tested to remove the laser energy from the process. It could be shown that a high defocusing of the optic system above 40 mm with a resulting beam diameter > 2.9 mm in a short overlap length of approx.
20 mm leads to the formation of a cup-shaped weld seam, which is preferred for avoidance of cracks and pores in the end crater. A laser optics with motor-driven lens system was used for the welding experiments to defocuse the laser beam without changing the position of the arc.
The transport phenomena in the wire feed laser beam welding are investigated numerically. A three-dimensional transient heat transfer and fluid flow model coupled with free surface tracing and element transport is developed. A ray-tracing method with local grid refinement algorithm is used to calculate the multiple reflections and Fresnel absorption on the keyhole wall. The filler material flows backward along the lateral side of the weld pool, and subsequently flows forward along the longitudinal plane. The occurrence of the bulging phenomenon may further prevent the downward transfer of the additional elements to the root of the weld pool.
Understanding the correlation between the morphological and functional properties of particulate materials is crucial across all fields of physical and natural sciences. This manuscript reports on the investigation of the effect of polyethylene glycol (PEG) employed as a capping Agent in the synthesis of SrTiO3 crystals. The crucial influence of PEG on both the shape and size of the strontium titanate particles is revealed, highlighting the effect on the photocurrents measured under
UV–Vis irradiation.
A new metallosilicate based on yttrium was synthesized and characterized by XRD, FT-IR, 29Si MAS-NMR, and 89Y MAS-NMR. The mixed framework of the material was confirmed by the detection of distinct chemical shift groups using 29Si MAS-NMR (at -82 to -87 ppm, -91 to -94 ppm, -96 to -102 ppm, and -105 to -108 ppm), as well as four distinct chemical shifts in the 89Y MAS-NMR spectrum (at -89, -142, -160, and -220 ppm). Adsorption and kinetic analyses indicated the potential of the new material for the removal of lead and cadmium from aqueous media. The adsorption results for lead indicated that dynamic equilibrium was reached after five hours, with total lead removal of around 94 %, while for cadmium it was reached in the first hour, with total Cadmium removal of around 74 %. The adsorptions of lead and cadmium were modeled using pseudo-first order (PFO) and pseudo-second order (PSO) kinetic models. Although both models provided high R2 values (0.9903 and 0.9980, respectively), the PSO model presented a much lower χ2 red value (4.41×10−4), compared to the PFO model (2.12×10−3), which indicated that the rate-limiting step was probably due to the chemisorption of lead from the solution onto the yttrium-based metallosilicate.
To improve the predictive capability of long-term stress relaxation of elastomers during thermo-oxidative ageing, a method to separate reversible and irreversible processes was adopted.
The separation is performed through the analysis of compression set after tempering. On the Basis of this separation, a numerical model for long-term stress relaxation during homogeneous ageing is proposed. The model consists of an additive contribution of physical and chemical relaxation.
Computer simulations of compression stress relaxation were performed for long ageing times and the results were validated with the Arrhenius treatment, the kinetic study and the time-temperature superposition technique based on experimental data. For chemical relaxation, two decay functions are introduced each with an activation energy and a degradative process. The first process with the lower activation energy dominates at lower ageing times, while the second one with the higher activation energy at longer ageing times. A degradation-rate based model for the evolution of each process and ist contribution to the total system during homogeneous ageing is proposed. The main advantage of the model is the possibility to quickly validate the interpolation at lower temperatures within the range of slower chemical processes without forcing a straight-line extrapolation.
High Entropy Alloys (HEAs) are a recent class of materials. In contrast to conventional alloys, HEAs consist of five alloying elements in equiatomic equilibrium. The high entropy effect is due, among other things, to the increased configuration entropy, which promotes solid solution formation. Many HEAs have enormous application potential due to excellent structural property combinations from very low to high temperatures. For the introduction of HEAs in real components, however, the question of the applicability of machining production technologies for component manufacture is of central importance. This has so far received Little attention in global materials research. Reliable and safe processing is essential for the demand of economical component production for potential areas of application, e.g. in power plant technology.
For metals, milling is the standard machining process. This article presents the results of machining analyses. It focuses on the surface integrity resulting from the milling process on a Co20Cr20Fe20Mn20Ni20-HEA. For this purpose, investigations were carried out using ball nose end milling tools for conventional milling process in comparison to an innovative hybrid process available at BAM Berlin, Ultrasonic-Assisted Milling (USAM). USAM promises a lower Degradation of the surface properties due to lower loads on the workpiece surface during machining.
For this purpose, basic milling parameters (cutting speed and tooth feed) were systematically varied and cutting forces were measured during the milling experiments. The subsequent Analysis of these forces allows an understanding of the mechanical loads acting on the tool and component surface. These loads cause topographical, mechanical and microstructural influences on the surface and consequently on the surface integrity. For their characterization, light and scanning electron microscopy were used, and the roughness and residual stresses via X-ray diffraction were measured. The results indicate significant advantages using USAM, especially due to reduced cutting forces compared to the conventional milling process. This causes lower mechanical loads on the tool and surface, combined with lower tensile residual stresses on and below the surface, and ultimately results in a significantly enhanced surface integrity.
The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed.
The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed.
Im DGMK-Projekt 780 wurde eine forcierte Prüfmethode entwickelt zur Bestimmung der Beständigkeit von metallenen Werkstoffen gegenüber Brennstoffen aus Mitteldestillaten und Gemischen aus Mitteldestillat und paraffinischen Kohlenwasserstoffen, die jeweils Fettsäuremethylester (FAME) als biogene Komponente enthalten. Bei der Prüfmethode werden Proben des Werkstoffes in einem speziellen Prüfmedien ausgelagert. Die Zusammensetzung von zwei Prüfmedien wurde im Vorhaben erarbeitet. Die Prüfmedien decken für den FAME-Anteil einen Bereich von bis zu 20 % (V/V) ab. Die Auslagerung kann bei geringem Aufwand unter Atmosphärendruck durchgeführt werden.
Die Eignung einer Auswahl von metallenen Werkstoffen und Polymerwerkstoffen, die für Versorgungsanlagen für Mitteldestillat relevant sind, wurde durch Auslagerung in folgenden nicht gealterten Brennstoffen bestimmt: Heizöl EL schwefelarm (B0), Heizöl EL schwefelarm mit 20 % (V/V) FAME (B20), FAME (B100) und hydriertes Pflanzenöl (HVO). Die Temperatur bei der Auslagerung betrug 50 °C für die metallenen Werkstoffe und 40 °C und 70 °C für die Polymerwerkstoffe. Die Ergebnisse der Beständigkeitsbewertung wurden in Beständigkeitslisten zusammengefasst. Die mit dem B20 erhaltenen Werkstoffbeständigkeiten gelten generell für Gemische aus Heizöl EL schwefelarm und FAME mit einem FAME-Gehalt bis zu 20 % (V/V). Sie sind auch auf Gemische aus Dieselkraftstoff und FAME mit einem FAME-Gehalt bis 20 %(V/V) übertragbar.
Die forcierte Prüfmethode kann insbesondere KMUs bei der Weiterentwicklung von bestehenden Produkten und der Entwicklung von neuen Produkten als ein kostengünstiger Schnelltest zur Überprüfung der Werkstoff- und Bauteilbeständigkeit gegenüber Mitteldestillaten mit hohem FAME-Anteil dienen. Sie kann für die Hersteller die Sicherheit erhöhen, dass Bauteile die Freigabeprüfungen der Bauaufsicht bestehen, wobei die Freigabe aber nur für Deutschland gültig ist.
Die Erkenntnisse des Forschungsvorhabens können in eine harmonisierte Europäischen Norm für alternative Brenn- und Kraftstoffe einfließen. Diese ist für die Bauteilhersteller die Voraussetzung für die Erschließung des europäischen Marktes.
Recent studies have confirmed the widening of the weld pool interface, known as a bulge effect, during deep penetration high power laser beam welding. The link between such geometric particularities of the weld pool shape and the hot cracking phenomena is significant. The present work seeks to extend the level of understanding by investigating their relationship. A coupled multiphysics, multiscale numerical framework is developed, comprising a series of subsequent analyses. The study examines the influences of the bulge on the three most dominant effects causing hot cracking, namely the thermal cycles, the mechanical loading, and the local microstructure. The bulge in the weld pool shape forms approximately in the middle of the plate, thus correlating with the location of hot cracking. It increases the hot cracking susceptibility by enhancing the three dominant effects. The numerical results are backed up by experimental data.
The development of high energy laser sources enables single-pass welds of thick plates up to 30 mm, but often additional materials are needed to influence the properties of the weld seams. However, the homogenous distribution of filler materials in form of e.g. electrodes is only possible up to 7 mm while the elements are only traceable up to a depth of 14 mm. To overcome this problem a two-step process is used where first the edges of the weld partners are coated with the filler material by laser metal deposition (LMD) and afterwards are welded by laser beam. Single-pass welds with electromagnetic weld pool support of 30 mm thick S355 J2+N-plates with austenitic AISI 316L-coatings were investigated as well as the influence of the coatings to the penetration depth of the laser beam without electromagnetic weld pool support in double-sided joints. The weld seams were tested by X-ray inspection and cross sections.
Polyaniline/Silicon Dioxide Composite-Based Coating for Corrosion Protection in Geothermal Systems
(2020)
Geothermal energy is one of the cleanest renewable alternatives to reduce the dependency on fossil fuel [1, 2]. Despite its promising future, its implementation faces various challenges, one of them being corrosion processes. To implement this energy, hot fluids are pumped from a geothermal well. These hot fluids originate from deep within the earth, so consist of different ionic species and gases in a wide range of temperatures, which lead to their corrosive nature. In terms of geothermal energy resources, Indonesia is at the forefront, with the highest preserved geothermal energy in the world of about 29 GWe and 312 potential geothermal locations [3]. Geothermal wells in Sibayak (North Sumatera), Indonesia, belong to young stratovolcanoes and have operating temperatures varying from 36 °C at the near ground surface to 310 °C at the bottom of the well, which is liquid-dominated with acidic and saline properties [4, 5]. Therefore, this geothermal fluid creates an aggressive environment that is conducive to corrosion of the powerplant infrastructure.
Parts of the geothermal powerplant infrastructure, such as pipelines and heat exchangers, are commonly made of metals, e.g. carbon steel and stainless steel. Consequently, they may undergo corrosion and scaling when exposed to the geothermal fluid, especially for carbon steel. To ensure the safety and longevity of a geothermal powerplant, the infrastructure is constructed of expensive corrosion resistant alloys [6–10], e.g., titanium and Ni-Cr based alloys, or carbon steel which needs to be protected by coatings or inhibitors.
To address the corrosion of carbon steel in the geothermal environment, artificial geothermal water was used to simulate a geothermal well in Sibayak, Indonesia, with pH 4 and a saline composition of 1,500 mg/l Cl-, 20 mg/l SO42-, 15 mg/l HCO3-, 200 mg/l Ca2+, 250 mg/l K+, and 600 mg/l Na+. Carbon steel underwent the most severe corrosion at 150°C in an oxygen-containing solution with a corrosion rate of 0.34 mm/year, which is approximately ten times higher than that in the absence of dissolved oxygen. In all conditions, pitting corrosion was observed, which necessitate a protection strategy on carbon steel. In order to promote a cost effective and locally available option, this work focused on an easily applicable coating which utilized local resources.
Toward developing such protective coating based on the locally available resources in Indonesia which can yield good corrosion resistance and thermal stability in geothermal environment, two additional components, i.e. polyaniline (PANI) and silicon dioxide, were used to modify an alkyd-based commercial coating. The selection of the alkyd-based coating as a matrix focused on the industrial convenience basis, where the coating application procedure should be simple and easy to apply within reasonable costs. The alkyd-based coating underwent severe blistering when exposed to the artificial geothermal water at 70 and 150°C due to the reaction between CaCO3 (as one of its components) and the artificial geothermal water, as well as a possible alkyd hydrolysis in the initial stage of exposure. In the oxygen-free solution, the degradation was controlled by chemical and thermal reactions, whereas in the aerated condition, oxidization at the coating surface further accelerated polymer degradation.
PANI was chosen as one of the anticorrosion pigments which was widely developed over the past decades. To investigate the interaction between PANI and the artificial geothermal water, PANI film was electrochemically deposited on the carbon steel surface and exposed to the artificial geothermal water. Electrochemically synthesized oxalate-doped PANI was protective against corrosion of carbon steel in artificial geothermal water at room temperature. The mechanism involved an exchange of electroactive species within the coating layer, as confirmed by electrochemical impedance spectra. Interaction of ionic species, such as Cl-, Na+, Ca2+ from the artificial geothermal water, with the outer layer of PANI is suggested both at 25°C and 150°C, based on the EDX spectra of the coating surface after exposure to the artificial geothermal water. Thus, the protection mechanism of PANI is not solely based on the physical barrier layer properties, but rather associated with the redox mediated properties of PANI, which selectively allow ionic species intrusion from the electrolyte into the PANI layer. Although PANI is a promising candidate as an anticorrosion coating, its morphological characterization reveals that electrochemically deposited PANI is not stable for an application at 150°C. Therefore, another approach was used to promote better protective behavior of PANI by dispersing chemically synthesized PANI in the alkyd-based coating.
To enhance the thermal stability of the coating, silicon dioxide (SiO2) was added, which was able to prolong the sustainability of coated metals until 28 days compared to the unmodified alkyd-based coating, which underwent a change in color to brown/orange only within 7 days of exposure. This improvement might be associated with the role of SiO2 to proportionate the thermal expansion coefficient of the coating system to be compatible with that of carbon steel. Although the coating is thermally enhanced, the electrolyte might still intrude through the coating resulting in the change of coating color after 28 days of exposure in the artificial geothermal water. When PANI was added, the coating system provided an active corrosion protection on the carbon steel surface. The chemical and morphological characterization of the PANI-alkyd and SiO2-alkyd coating system showed that coatings were improved, and no blisters were observed, albeit the degradation continued. Based on the results of exposure tests, the combined coating system was further investigated.
The combinational coating of PANI/SiO2-alkyd was used with 2 wt% of PANI and 15 wt% of SiO2. Electrochemical tests indicated cathodic protection at 150°C, as the Ecorr of PANI/SiO2 remained approximately 400 mV lower than the carbon steel potential. The impedance spectra of the combinational coating of PANI/SiO2 showed a continuous decrease in the absolute impedance value over time. A significant decrease was observed within one day of exposure, followed by a slow gradual decrease, which might be associated with water absorption in the coating. FTIR spectra revealed that several peaks associated with the organic portion of the coatings were reduced after the specimens were exposed for 6 months. However, the absorption peaks related to the inorganic portion of the coatings remained stable until 6 months. Morphological characterization of the combinational coating of PANI/SiO2 showed that there were no blisters or significant discoloration of coatings after long-term exposure for 6 months in artificial geothermal water at 150°C, indicating that the chemical degradation does not significantly affect the functionality of the coating. This clearly shows the durability of PANI/SiO2 coating in the geothermal condition, suggesting that this coating can be used for such geothermal application. However, further testing of this coating should be conducted in a real geothermal environment on-site to ensure safety and viability.
We present an approach towards the in situ solid state NMR monitoring of mechanochemical reactions in a ball mill. A miniaturized vibration ball mill is integrated into the measuring coil of a home-built solid state NMR probe, allowing for static solid state NMR measurements during the mechanochemical reaction within the vessel. The setup allows to quantitatively follow the product evolution of a prototypical mechanochemical reaction, the formation of zinc phenylphosphonate from zinc acetate and phenylphosphonic acid. MAS NMR investigations on the final reaction mixture confirmed a reaction yield of 89% in a typical example. Thus, NMR spectroscopy may in the future provide complementary information about reaction mechanisms of mechanochemical reactions and team up with other analytical methods which have been employed to follow reactions in situ, such as Raman spectroscopy or X-ray diffraction.
Die Eigenschaften verschiedener Werkstoffe werden behandelt und typische Werkstoffkennwerte angegeben. Es werden Arten der Beanspruchung von Bauteilen und Werkstoffen vorgestellt, die diese in technischen Anwendungen unterworfen sind. Im Betrieb von Bauteilen kann Materialschädigung und unter Umständen auch Versagen eintreten. Mögliche Mechanismen und Ursachen werden erläutert und Einblicke in die Methodik der Schadensanalyse gegeben.
A heat treated glass that formed crystals under controlled conditions can be a glass ceramic. A proper understanding of crystallization in glassy melts is needed yet still lacking. Involved processes include the mobility of Elements within the glass during heat treatment and the reorganization of atomic bonds during crystallization. This change in coordination number of certain elements is easily observable in bulk glass samples during heat treatment with XAS. Our plan was to monitor these reorganization processes in situ at the immediate surface during heat treatment with PEEM to get time and spatial resolved data.
A summery of previous research regarding surface crystallization is given as well as results regarding thecurrent DFG project are presented.
As opposed to reviewing results on experimental determination of residual stress by diffraction, this paper discusses the open issues when dealing with residual stress determination in additive manufactured parts, in particular those manufactured with laser powder bed fusion techniques. Three points are addressed in detail: (a) the proper determination of the strain-free reference d0, (b) the problem of the determination of the principal axes, and (c) the use of the correct diffraction elastic constants. It is shown that all methods to determine the strain-free reference d0 suffer from caveats, and care must be taken in evaluating the most suitable for the problem being tackled. In addition, it is shown that, in some systems, the principal axes do correspond to the geometrical axes of the specimen, but this needs to be systematically checked, especially in the case of uni- or bidirectional hatching strategies. Finally, the need to experimentally determine the proper diffraction elastic constants is underlined, especially in the case of strongly textured specimens, which again depends on the deposition strategy.
Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles in the frame of the European project nPSize - Improved traceability chain of nanoparticle size measurements. SEM Image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328.
Nanotechnology and lasers are among the most successful and active fields of research and technology that have boomed during the past two decades. Many improvements are based on the controlled manufacturing of nanostructures that enable tailored material functionalization for a wide range of industrial applications, electronics, medicine, etc., and have already found entry into our daily life. One appealing approach for manufacturing such nanostructures in a flexible, robust, rapid, and contactless one-step process is based on the generation of laser-induced periodic surface structures (LIPSS). This Perspectives article analyzes the footprint of the research area of LIPSS on the basis of a detailed literature search, provides a brief overview on its current trends, describes the European funding strategies within the Horizon 2020 programme, and outlines promising future directions.
This paper investigates fast and inexpensive measurement methods for defect detection in parts produced by Additive Manufacturing (AM) with special focus on lattice parts made of ceramics. By Lithography-based Ceramic Manufacturing, parts were built both without defects and with typical defects intentionally introduced. These defects were investigated and confirmed by industrial X-ray Computed Tomography. Alternative inexpensive methods were applied afterwards on the parts such as weighing, volume determination by Archimedes method and gas permeability measurement. The results showed, that defects resulting in around 20% of change in volume and mass could be separated from parts free of defects by determination of mass or volume. Minor defects were not detectable as they were in the range of process-related fluctuations. Permeability measurement did not allow to safely identify parts with defects. The measurement methods investigated can be easily integrated in AM process chains to support quality control.
Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. SEM image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328.
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed.
Understanding the failure mechanisms that lead to leakage of rubber seals at low temperatures is important. Rubber properties are highly temperature dependent. Changes in behaviour at low temperatures can result from the rubber-glass transition and for some rubbers by partial crystallisation. Experimental results on the low temperature behaviour of different rubber seals were discussed to help understand seal failure processes.
A self-restraint hot cracking test (free edge test) was used in combination with a novel optical measurement technique to determine the critical straining conditions for solidification cracking for the stainless steel grade 1.4828 (AISI 309). The Lucas-Kanade algorithm for the optical flow (OF) calculation was implemented to obtain the full-field displacement and then the full-field strain.
The use of external laser illumination with appropriate filters allows to obtain good image quality with good contrast. The critical straining conditions required for solidification cracking can be obtained by means the proposed technique in the immediate vicinity of the solidification front. A very good repeatability was demonstrated for the used measurement technique. The critical straining conditions for solidification cracking for the tested steel und under this welding conditions has been detected