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Paper des Monats
- ja (32)
Tuff ist in vielen historischen Objekten in Deutschland verbaut, hat aber wegen seiner Porosität und hygrischen Eigenschaften eine schlechte Verwitterungsresistenz. Ziel des Vorhabens ist die Entwicklung eines gesteinsmehlmodifizierten Schutzsystems auf Kieselsäurebasis (GEMOSK) zur Konservierung verbauter Tuffe. Für die Schutzmittelherstellung wird eine geeignete Mischung aus Kieselsol und feinen Gesteinsmehlen aus Steinbruchrückständen und Tuffabfällen verwendet. Bei erfolgreichem Abschluss des Projektes kann GEMOSK im Denkmalpflegebereich eingesetzt werden. Dadurch werden die Bausubstanz besser erhalten, Tuffsteinressourcen eingespart und Tuffabfälle wiederverwertet.
In summary, we report a highly modular solid TTA-UC system comprising of a crystalline, thermally stable PCN222(Pd) MOF with CA-coated MOF channels and with a DPA annihilator embedded in a solution-like environment in the MOF channels. This solid material displays blue upconverted delayed emission with a luminescence lifetime of 373 us, a threshold value of 329 mW*cm-2 and a triplet–triplet energy transfer efficiency of 82%. This optical application adds another facet to the versatile chemistry of PCN-222 MOFs. The design concept is also applicable to other TTA-UC pairs and enables tuning of the UCL color, for example, by replacing DPA with other dyes as exemplarily shown for 2,5,8,11-tetra-tert-butyl-perylene, that yields UCL at 450 nm. Current work aims to reduce the oxygen sensitivity and to increase the retention of the trapped annihilators in organic environments, for example, by tuning the chain length of the carboxylic acid and by coating the MOF surface. In addition, the TTA-UC efficiency will be further enhanced by reducing the reabsorption of the UC emission caused by Pd(TCPP) and by optimizing the sensitizer/annihilator interface.
Das DED Auftragschweißen ist ein additives Fertigungsverfahren für Metalle, bei dem das Material schichtweise auf ein Substrat aufgetragen wird. Die schnellen Temperaturzyklen rufen Spannungsgradienten im Bauteil hervor. Der schichtweise Aufbau der Bauteile verursacht eine anisotrope Mikrostruktur. Mittels nachgelagerter Wärmebehandlung können diese Effekte verringert werden. Im anschließenden Schritt der Prozesskette wird das additiv hergestellte Bauteil mittels Drahterodieren von dem Substrat abgetrennt.
In diesem Beitrag wird eine thermo-mechanische Simulation der gesamten Prozesskette vorgestellt, welche den additiven Aufbau, Wärmebehandlung und das Abtrennen vom Substrat beinhaltet. Anstelle der in der Literatur üblichen schichtweisen Modellierungsstrategie für die DED Simulation wird das gesamte Bauteil in einem Stück vernetzt und der vollständig transiente, schichtweise Materialauftrag über Elementgruppen realisiert. Im Gegensatz zu früheren Simulationen muss der nichtlineare Kontakt zwischen den Schichten nicht berücksichtigt werden, was die Rechenzeiten deutlich verkürzt.
Das Modell wurde validiert mittels Abgleiches des Verzugs aus Simulation und Experiment.
Die Proben, bestehend aus DIN 1.4404 (AISI 316L), wurden nach jedem Prozessschritt 3D gescannt um den Verzug zu quantifizieren. Zusätzlich wurden Querschnitte und Härtetests nach Vickers von unterschiedlich behandelten Proben durchgeführt, um den Effekt der Wärmebehandlung auf die Mikrostruktur und die Härte des Bauteils zu untersuchen.
Das Fügeverfahren Kleben bietet viele Vorteile, wie z.B. das Verbinden unterschiedlicher Materialklassen, geringe thermische Belastung (und damit ggf. verbundene Strukturveränderung/-schwächung) der Fügeteile und eine Lastverteilung über den gesamten Fügebereich. Die Auswahl an verfügbaren Klebstoffen und Vorbehandlungsoptionen sind dabei - wie die Applikationen auch - vielfältig. Es werden vier Applikationsbeispiele zu Referenzklebverbunden aus Edelstahl, zur Plasmaaktivierung von Niedrigenergie-Polymeren, zur Bestimmung der Haftfestigkeit von Lackierungen auf GFK und zur Wirkung von Primern vorgestellt. Einige Polymere weisen z.B. Eigenschaften auf, die eine Herstellung von festen und dauerhaft beanspruchbaren Kleb-verbindungen erschweren. Im Allgemeinen geht dies mit geringen Oberflächenenergien einher. Mittels Oberflächenvorbehandlung, z.B. durch Plasmafeinreinigung bzw. Plasmaaktivierung, können die Grenzflächen solcher Polymere - bezogen auf die Eignung als Fügeteile (Klebfestigkeit) oder als Substrat (Haftfestigkeit) – optimiert bzw. die Oberflächenenergie erhöht werden. Schnelle, zuverlässige und statistisch abgesicherte Prüfverfahren zur Ermittlung von Verbund-eigenschaften sind dabei unverzichtbar.
Challenges in Traceable Size Measurement of Non-Spherical, Non-Monodisperse Nanoparticles - nPSize
(2019)
Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary.
The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering.
Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs.zeige mehr
When assessing the performance of welded components residual stresses are vital. The possibilities of transferring the real boundary conditions of welding, which influence the residual stress, into the laboratory are highlighted in this contribution. The potentials of a test system specially developed for this purpose are demonstrated. The component design induces global process-, geometry- and material-dependent stresses, which can be simulated and quantified in the system. In addition, the resulting local residual stress distribution can be exactly determined with high spatial resolution with the aid of X-ray diffraction. Examples are presented of how the conditions to be found during production are simulated in the laboratory.
Die Präsentation gibt einen Überblick bezüglich der von der BAM im Rahmen des SimCoLas Verbundprojekts durchgeführten Arbeiten zum Thema "Photonische Prozessketten". Die numerisch abgebildete Prozesskette Tiefziehen/Laserstrahlschweißen wird darsgestellt und diskutiert. Fokus der Diskussion ist die entwickelte Methodik zur konsistenten Abbildung numerischer Prozessketten mit der Applikation Heissrisskritikalität beim Laserstrahlschweißen.
Der Vortrag gibt einen Überblick über Arbeiten im Rahmen der Themenstellung "photonische Prozessketten" des SimCoLas Projekts. Es werden Ergebnisse zur Datendurchgängigkeit der Prozesskette Umformen/Laserstrahlschweißen sowie erste Ergebnisse zu numerischen Schweißstruktursimulationen zur Bewertung der Heissrisskritikalität eines tiefgezogenen Napfes beim Laserstrahlschweißen gegeben.
The potential of lowered surface features as well as the application of wear resistant coatings have been known for many years to improve the tribological behavior of forming tools. More recent studies also discuss the capability of protruded microfeatures for adjusting the tribological behavior between contacting surfaces. The demand for a high wear resistance of such structures as well as their economical and reliable production, however, often limits the industrial application. The laser implantation process can overcome these limitations. In contrast to conventional cw-laser dispersing processes, where the formation of uniform metal matrix composite layers is intended, this surface engineering technique aims to improve the tribological behavior of contacting surfaces by a localized dispersing of pre-placed hard ceramic particles. This enables the formation of deterministic textures composed of separated wear resistant dome- or ring-shaped microstructures (implants).
Since TaC shows very promising material properties for improving the wear resistance of tools exposed to severe operating conditions, this paper analyzes its suitability for pulsed laser implantation on X38CrMoV5-3 tool steel for the first time. In the experiments, the influence of the particles and the laser parameters (pulse power, pulse duration and focal diameter) on the material properties of the localized dispersed zones was studied by optical microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction. The composite´s (micro-) hardness was measured and calculated by using a rule of mixture. Additionally, the influence of the laser parameters and the TaC particles on the geometrical properties of the implants was studied by optical microscopy and white light interferometry.
The results showed that defect-free implants with hardness values of ~900 HV1 can be obtained at the focal spot, since a localized dispersing of the TaC particles is possible using a pulsed millisecond laser. However, in dependence of the laser intensity, also a partial dissolution of the initial particles occurs. This leads to the precipitation of new dendritic TaC nanoparticles and to varying contents of retained austenite in the matrix. Both effects have a strong influence on the implant hardness and must be considert by the rule of mixture. Regarding the geometrical response it was pointed out that protruded microfeatures with heights up to 10 µm can be created. In comparison to laser remelted zones, the implanted zones showed significantly altered weld pool profiles due to the influence of the particles on the melt convection. A transition of the implant shape from predominantly dome-shaped to predominantly ring-shaped was observed for intensities >1.7∙106 W/cm2 due to the onset of the keyhole effect.
Diese Arbeit beschäftigt sich mit den Eigenschaften der photonenzählenden und spektralauflösenden Detektortechnik und möglichen Anwendungsgebieten in der zerstörungsfreien Prüfung. Dabei wurden konventionelle und photonenzählende Detektortechniken hinsichtlich der Bildqualität und Anwendbarkeit bei unterschiedlichen Prüfaufgaben verglichen und untersucht, inwiefern sich die Energieschwellwertsetzung auf die erreichbare Bildqualität und eine Materialdiskriminierbarkeit bei verschiedenen radiographischen Verfahren auswirkt.
Anhand von Anwendungsbeispielen wurden diese Eigenschaften und deren Auswirkung auf das Messergebnis analysiert. Neben der Radiographie wurden auch dreidimensionale Verfahren wie CT und Laminographie berücksichtigt.
Als eine der wichtigsten Eigenschaften der photonenzählenden Detektortechnik wurden zunächst die Energieauflösung des photonenzählenden Detektors und die Homogenität der Energieantwort über größere Detektorbereiche bestimmt. Dabei stellte sich heraus, dass die Energieauflösung eines abgegrenzten Detektorbereichs ca. 32 % bei 60 keV beträgt und die Streuung in der Energieantwort der einzelnen Detektorbereiche ca. 12 % ausmacht, woraus sich eine Gesamtunsicherheit in der spektralen Detektorantwort von ca. 44 % ergibt. Die geringe Energieauflösung und das stark heterogene Verhalten der Detektorbereiche ergeben sich vor allem aus der Detektorelektronik, welche nur eine globale Energieschwellwertsetzung zulässt.
Trotz dieser Einschränkungen konnte demonstriert werden, dass auch konventionelle radiographische Verfahren, wie Radiographie oder CT, vom Einsatz der photonenzählenden Technik profitieren. So ist es mit dieser Technik möglich, bei sehr geringen Dosisleistungen (z.B. aufgrund der Durchstrahlung großer Wandstärken von dichten Materialien) noch sehr gute Bildqualitäten zu erreichen. Die hohe Dynamik und Kontrastempfindlichkeit dieser Technik begünstigen die Inspektion von Leichtbauwerkstoffen wie Faserverbunde, was anhand von Vergleichen mit herkömmlicher Detektortechnik und anderen ZfP-Verfahren gezeigt werden konnte. Daneben konnte durch den Einsatz der Energieschwellwertsetzung der Einfluss von nicht bildzeichnender Streustrahlung im Röntgenbild um bis zu 20 % reduziert werden. Die Auswirkungen von Aufhärtungseffekten in der CT konnten sogar um bis zu Faktor 1 000 (in der mittleren quadratischen Abweichung), im Vergleich zu herkömmlicher Detektortechnik, reduziert werden.
Der Einsatz von photonenzählender Detektortechnik mit Röntgenblitzröhren ist hingegen nicht sinnvoll, da aufgrund der hohen Photonendichte pro Puls und einer endlichen Totzeit des Detektors in der Größenordnung der Pulsbreite eines Blitzes nur ein geringes Signal detektiert werden kann.
Im Hinblick auf eine Materialdiskriminierbarkeit konnte demonstriert werden, dass im Fall einer Radiographie anhand der Energieschwellwertsetzung im Detektor eine materialstärkenunabhängige Diskriminierung zwischen zwei Materialien (hier: Al und Fe) erzielt werden kann. Unter Einsatz mehrerer Energiefenster und eines Verfahrens der explorativen und multivariaten Datenanalyse konnte eine materialaufgelöste CT eines Multi-Material-Phantoms erreicht werden, wobei die Schwächungskoeffizienten der enthaltenen Materialien im relevanten Energieberiech teilweise sehr dicht beieinander lagen.
Neben Radiographie und CT wurde auch die Möglichkeit einer materialaufgelösten Laminographie am Beispiel eines glasfaserverstärkten Rotorblatts untersucht. Anhand der Energieschwellwertsetzung war nicht nur eine eindeutige Trennung der Glasfasern von der Epoxidharzmatrix möglich, sondern auch eine signifikante Reduzierung der durch die Laminographie entstandenen Artefakte. Der damit verbundene Gewinn an Information führt zu einer verbesserten Aussagefähigkeit des Untersuchungsergebnisses, was letztendlich eine gesteigerte Betriebssicherheit zur Folge hat.
Laser beam welding of aluminum die casting is challenging. A large quantity of gases (in particular hydrogen) is absorbed by aluminum during the die-cast manufacturing process and is contained in the base material in solved or bound form. After re-melting by the laser, the gases are released and are present in the melt as pores. Many of these metallurgic pores remain in the weld seam as a result of the high solidification velocities. The natural (Archimedean) buoyancy is not sufficient to remove the pores from the weld pool leading to process instabilities and poor mechanical properties of the weld. Therefore, an electromagnetic (EM) system is used to apply an additional buoyancy component to the pores. The physical mechanism is based on the generation of Lorentz forces, whereby an electromagnetic pressure is introduced into the weld pool. The EM system exploits the difference in electrical conductivity between poorly conducting pores (inclusions) and the comparatively better conducting aluminum melt to increase the resulting buoyancy velocity of the pores. Within the present study, the electromagnetic supported degassing is investigated in dependence on the laser beam power, welding velocity and electromagnetic flux density. By means of a design of experiments a systematic variation of these parameters is carried out for partial penetration laser beam welding of 6 mm thick sheets of wrought aluminum alloy AlMg3 and die-cast aluminum alloy AlSi12(Fe) where the wrought alloy serves as a reference. The proportion of pores in the weld seams is determined using X-ray images, computed tomography (CT-) images and cross-section images. The results prove a significant reduction of the porosity up to 70 % for both materials as a function of the magnetic flux density
The paper describes a systematic investigation of the EM influenced laser beam welding of the aluminum die casting alloy AlSi12(Fe) in comparison to a reference material, a wrought aluminum alloy AlMg3. By using of a face centred CCD test plan, the influencing variables laser power, welding velocity and magnetic flux density are varied with regard to their influence on the remaining porosity. The global pore fraction of the weld seams was analyzed by X-ray images with ImageJ. This enabled a qualitatively very good regression model to be derived for the respective material, which identifies the dominant influencing variables. The results prove, statistically verified, for the investigated parameter range, that
- the magnetic flux density is the main cause for the porosity reduction,
- the porosity rises with increasing laser power the porosity in the weld seams rises,
- the influence of the welding velocity is negligible,
- the pore quantity in wrought alloy is more strongly minimized by the magnetic flux density than in die casting,
- the porosity decreases due to the EM influence by approx. 70 % compared to the unaffected welds. This effect is emphasized by the contour line charts, which illustrate the relationship between laser power and magnetic flux density.
With the exception of the quadratic influence of B at the wrought alloy, the statistical correlation shows a linear development of the respective influence variables for both aluminum alloys. In order to investigate these deviations, further simulations with a focus on weld pool geometry and weld pool flow are to be performed. In addition, the welding results can be classified in accordance with DIN EN ISO 13919-2 in the highest evaluation group B for AlMg3 and in evaluation group C for AlSi12(Fe) by applying a magnetic flux density of 350 mT. The analysis of the CT images at constant laser power and welding velocity allows a direct comparison both between the two alloys and also as a function of the magnetic flux density with regard to the number and size of pores. An increase in the magnetic flux density leads to a significant decrease in the number and volume of pores, which can be seen more clearly in wrought alloy than in die casting. Very acceptable results can be achieved for both materials and different welding parameters. This successfully demonstrates the desired process robustness and functionality of the EM system for practical applications. For subsequent investigations of overlap joints, the lowest possible laser power and a high magnetic flux density are recommended.
Friction stir welding (FSW) of high-melting temperature alloys, such as steel and Inconel, requires tooling that can survive under the applied loads at the elevated temperatures. Tungsten-Rhenium (W-Re) alloys are a suitable candidate for this application; however, the costs typically associated with achieving the required densities and grain structure for the tooling are high due to the lengthy traditional processing required. Further costs are incurred in machining the starting bar stock to the final FSW tooling configuration. An alternate processing method is used in this study to shorten the fabrication time using direct current sintering which rapidly consolidates the starting powders at lower temperatures than used in traditional powder metallurgy. Although this process enables retention of the fine grain size, the sintering time is too short to form the desired single, solid phase. Therefore, the specimens were subjected to a post-consolidation heat treatment to fully solutionize the W matrix. Once the desired density and solid solution phase was verified in coupons, the final processing parameters were used to consolidate a net shape tool for FSW.
Diffraction-based experimental determination of Residual Stress in AM parts: A critical discussion
(2019)
Additive manufacturing (AM) technologies have experienced an exceedingly rapid growth, not always paralleled by the knowledge about the materials properties and performance. In particular, residual stress (RS) has been soon recognized as an issue in AM parts, so that parts are always post-heat-treated. Moreover, much effort has been spent on simulating RS, especially using finite element methods.
The experimental determination of RS has thereby become increasingly important, and even simple data constitute (to date) a piece of knowledge to fill the above-mentioned gap. In particular, diffraction methods, which are basically non-destructive, offer enormous possibilities to gain knowledge on real components, since neutrons and synchrotron radiation can penetrate even heavy metals up to several millimeters (or even centimeters). Indeed, some success has been obtained, and the knowledge about the origins of the RS fields, as well as their variation as a consequence of heat or mechanical treatments, has been greatly expanded.
In this talk, a few success stories will be outlined. It will be shown how the determination of RS in metallic parts (with focus on those produced by laser powder bed fusion) has even allowed showing that process parameters that were considered unimportant play a major role in the onset of stress.
However, while RS is starting to be considered in the part design, deposition strategy (e.g. build plate temperature), and even in the definition of the relevant metric to assess the quality of a part, much is still to be investigated about the hypotheses underlying its experimental determination. Therefore, some aspects to be aware of, or even to date unclear will also be discussed, such as the determination of the reference unstrained samples and of the principal axes of stress. All these aspects will draw the path towards a comprehensive understanding of the process-structure-performance relationships in AM materials and parts.
Thermal decomposition of (NH4)2[OsxPt1-xCl6] as single-source precursors for Os-Pt binary alloys has been investigated under ambient and high pressure up to 40 GPa. Thermal decomposition of mixed-metal (NH4)2[OsxPt1-xCl6] precursor in hydrogen atmosphere (reductive environment) under ambient pressure results in formation of β-trans[Pt(NH3)2Cl2] and α-trans-[Pt(NH3)2Cl2] crystalline intermediates as well as single and twophase Os—Pt binary alloys. For the first time, direct thermal decomposition of coordination compound under pressure has been investigated. A formation of pure metallic alloys from single-source precursors under pressure has been shown. Miscibility between fcc- and hcpstructured alloys has been probed up to 50 GPa by in situ high-pressure X-ray diffraction. Miscibility gap between fcc- and hcp-structured alloys does not change its positions with pressure up to at least 50 GPa.
The second edition of this textbook on physical electrochemistry, written by two experienced teachers of physical chemistry, corrosion engineering and materials science and engineering, covers the current knowledge which should be transferred to students of these fields.
In 20 chapters the fundamentals of electrochemistry, the most important electrochemical measurement techniques and applications of electrochemistry are covered.
It can be concluded that this study fulfills its intension of “serving as a key textbook in undergraduate courses” dealing with electrochemistry and being “a reference source for graduated students, researchers and engineers” interested in this field. Teachers will find sufficient content for preparing lectures on this topic. Even self‐learning is well supported by the clear structure, presented content and provided sources for further reading.
Dieser umfangreiche Leitfaden gibt Auskunft zur thermisch‐mechanischen Beständigkeit von 199 Eisen‐, 77 Nickelbasis‐ und 23 Kobaltbasislegierungen und ist ein sehr gutes und bestimmt erweiterbares Nachschlagewerk für Konstrukteure und Praktiker, die über den Einsatz geeigneter Werkstoffe in hohen Temperaturen entscheiden müssen.
The influence of heat input and welding speed on the microstructure and mechanical properties of single-pass hybrid laser arc welded 20mm thick plates of high-strength pipeline steel X120 were presented. The heat Input was varied in the range of 1.4 kJ mm−1 to 2.9 kJ mm−1, while the welding speed was changed between 0.5m min−1 and 1.5m min−1. A novel technique of bath support based on external oscillating electromagnetic field was used to compensate the hydrostatic pressure at low welding velocities. A major advantage of this technology is, that the welding speed and thus the cooling time t8/5 can be variated in a wide parameter window without issues regarding the weld root quality. The recommended welding thermal cycles for the pipeline steel X120 can be met by that way. All tested Charpy-V specimens meet the requirements of API 5 L regarding the impact energy. For higher heat inputs the average impact energy was 144 ± 37 J at a testing temperature of −40 °C. High heat Input above 1.6 kJ mm−1 leads to softening in the weld metal and heat-affected-zone resulting in loss of strength. The minimum tensile strength of 915 MPa could be achieved at heat inputs between 1.4 kJ mm−1 and 1.6 kJ mm−1.
The laser-based direct energy deposition (DED) as a technology for additive manufacturing allows the production of near net shape components. Industrial applications require a stable process to ensure reproducible quality. Instabilities in the manufacturing process can lead to faulty components which do not meet the required properties.
The DED process is adjusted by various parameters such as laser power, velocity, powder mass flow and spot diameter, which interact with each other. A frequently used comparative parameter in welding is the energy per unit length and is calculated from the laser power and the velocity in laser welding. The powder per unit length comparative parameter in the DED process has also be taken into account, because this filler material absorbs energy in addition to the base material.
This paper deals with the influence of mass energy as a comparative parameter for determining the properties of additively manufactured parts. The same energy per unit length of 60 J/mm as well as the same powder per unit length of 7.2 mg/mm can be adjusted with different parameter sets. The energy per unit length and the powder per unit length determine the mass energy. The laser power is varied within the experiments between 400 W and 900 W. Energy per unit length and powder per unit length are kept constant by adjusting velocity and powder mass flow. Using the example of Inconel 718, experiments are carried out with the determined parameter sets. In a first step, individual tracks are produced and analyzed by means of micro section. The geometry of the tracks shows differences in height and width. In addition, the increasing laser power leads to a higher dilution of the base material. To determine the suitability of the parameters for additive manufacturing use, the individual tracks are used to build up parts with a square base area of 20x20 mm². An investigation by Archimedean principle shows a higher porosity with lower laser power. By further analysis of the micro sections, it can be seen that at low laser power, connection errors occur between the tracks.
The results show that laser power, velocity and powder mass flow have to be considered in particular, because a constant mass energy can lead to different geometric as well as microscopic properties.
Current analyses show a widespread occurrence of microplastic particles in food products and raise the question of potential risks to human health. Plastic particles are widely considered to be inert due to their low chemical reactivity and therefore supposed to pose, if at all only minor hazards. However, variable physicochemical conditions during the passage of the gastrointestinal tract gain strong importance, as they may affect particle characteristics. This study aims to analyze the impact of the gastrointestinal passage on the physicochemical particle characteristics of the five most produced and thus environmentally relevant plastic materials polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate and polystyrene. Scanning electron microscopy (SEM) and subsequent image analysis were employed to characterize microplastic particles. Our results demonstrate a high resistance of all plastic particles to the artificial digestive juices. The present results underline that the main stages of the human gastrointestinal tract do not decompose the particles. This allows a direct correlation between the physicochemical particle characteristics before and after digestion. Special attention must be paid to the adsorption of organic compounds like proteins, mucins and lipids on plastic particles since it could lead to misinterpretations of particle sizes and shapes.
Ferritic spheroidal graphite cast iron (SGI) materials have a remarkable technical poten-tial and economic impact in modern industry. These features are closely related to the question of how the cast materials can be produced without structural defects and graphite degenerations such as for example chunky graphite. Although the chunky graphite degeneration superficially seems to be well known, its metallurgical background is still controversially discussed, appropriate field-tested non-destructive tools for its quantification in castings are lacking and the knowledge on its impact on material properties is fairly limited. Addressing this status, the article is providing a current overview on the subject. Existing theories on formation and growth mechanisms of chunky graphite are briefly reviewed. Furthermore, from a metallurgical point of view, causes for the appearance of chunky graphite as well as preventive measures are concisely summarized. Particular attention is paid to the morphology of chunky graphite and how it can be characterized by destructive and non-destructive techniques. Special emphasis was laid on providing a comprehensive overview on the impact of chunky graphite on strength, ductility, fatigue limit, fatigue crack growth rate as well as fracture tough-ness of ferritic SGI materials based on experimental data. Moreover, conclusions for the assessment of castings affected by chunky graphite are drawn.
Die zunehmenden Nachweise von Kunststoffen in verschiedenen Umweltmedien erfahren in den letzten Jahren weltweit ein zunehmendes wissenschaftliches, gesellschaftliches und politisches Interesse. Besondere Aufmerksamkeit erfahren Kunststoffpartikel von 1-1.000 µm sogenanntes Mikroplastik. Es wurde mittlerweile in Wasser, Böden, Luft und Biota nachgewiesen. Obwohl die Wirkungen auf die natürlichen Umweltfunktionen noch unklar sind und kontrovers diskutiert werden, ist allein durch die ubiquitäre Präsenz eine systematische Erfassung von Eintragsquellen und Verbleib der Partikel über alle Umweltmedien notwendig, um Maßnahmen zur Reduktion der Einträge zu veranlassen.
Für eine zuverlässige Erfassung sind medienübergreifende Verfahren zu entwickeln, welche die drei analytischen Schritte, Probennahme, Probenaufbereitung und Detektion beinhalten. Die Verfahren adressieren unterschiedliche Zielgruppen, welche verschiedene analytische Informationen fordern. Für die akademische Bewertung werden Verfahren mit hohem analytischen Aufwand favorisiert, welche möglichst detaillierte Information über Partikelsorte, -größe, -zahl und -oberflächenbeschaffenheit geben. Im Gegensatz dazu, fordern Anwender aus der Praxis schnelle und einfache Monitoring Verfahren, welche die Bestimmung eines Massengehaltes, bzw. eines Grenzwertes zulassen. Allen ist gemeinsam, dass ein hoher interdisziplinärer Anspruch besteht, der sowohl technische Voraussetzungen zur repräsentativen Probennahme und die Limitationen von Detektionsverfahren berücksichtigt, als auch die Fachkompetenz von Biologen, Umweltwissenschaften, Analytiker und Polymerwissenschaftler einschließt.
Verfahren zum Mikroplastiknachweis müssen auch verschieden Proben mit sehr unterschiedlichen Gehalten an natürlicher Matrix gerecht werden. So müssen allein für Wasser Verfahren entwickelt werden, die Mikroplastik verschiedener Form (sphärische Partikel, komplexe Bruchstücke, Fasern) aus Medien mit sehr variablen Partikelanteil (u.a. Trinkwasser, Oberflächenwasser, Abwasser) repräsentativ erfassen sowie schnell und kostengünstig sind – einschließlich der notwendigen Probenaufbereitung. Die jeweiligen Detektionsverfahren müssen z.B. einzelne Partikel oder integrale Gehalte über drei Dekadenklassen für thermoplastische und insbesondere auch elastomere Partikelsorten erfassen können.
Casks for storage and transportation of used fuel rods of radioactive material are equipped with polyethylene (PE) for improved neutron flux shielding. The embedded PE structures are additionally exposed to gamma radiation and heat flow due to the specific high activity of the fission products. 60Co γ-radiation and heat load experiments at 125°C has been performed to evaluate PE degradation during the ageing process. FAR-FTIR-experiments were subsequently performed at differently aged PE test samples to characterize the oxidation process and morphological changes in the samples during the ageing at 125°C.
Im Vortrag werden Ergebnisse eines Forschungsvorhabens des DVS vorgestellt, in dem ein Verfahren zur Vermeidung von Schweißimperfektionen im Überlappbereich einer laserstrahlhybridgeschweißten Rundnaht entwickelt wird. Die Strategie der Prozessführung beim Schließen der Rundnaht sieht hervor, dass ein fehlerfreier Überlappbereich durch die Kontrolle der Erstarrungsbedingungen am Schweißnahtende erreicht wird. Die kontrollierte Wärmeführung wird durch eine Anpassung der Parameter von beiden beteiligten Schweißprozessen, dem Laserstrahl- sowie MSG-Schweißprozess realisiert. Es konnte gezeigt werden, dass eine Defokussierung des Laserstrahls von bis zu 40 mm über den Weg von max. 15 mm während der Bewegung des Schweißkopfes zu einer deutlich besseren Nahtausbildung im Überlappbereich führt. Es konnte eine günstige kelchförmige Schweißnahtform ohne eine Tendenz zur Rissbildung erzielt werden.
Recent facade fires worldwide have driven change in regulations for façade fire safety in different parts of the world. The Grenfell Tower fire 2017 in London triggered a thorough investigation of many aspects of the fire. One investigation was about the UK building regulations from Dame Judith Hackett. This investigation compares the UK with the situation other parts of the world. Key findings of the review of building regulations by Judith Hackett are:
We report the synthesis and characterization of carbon nanodots (CDs) with high quantum yield (>50%) and tailored optical absorption as well as emission properties. A well-described protocol with polyethyleneimine (PEI) as amine precursor is used as a reference to a new CD system which is stabilized by aromatic 2,3-diaminopyridine (DAP) molecules instead. The DAP stabilizer is installed in order to red-shift the absorption peak of the n-π* electron transition allowing efficient radiative recombination and light emission. Size, shape, and chemical composition of the samples are determined by (HR)TEM, EDX and FTIR-spectroscopy. Optical parameters are investigated using UV-VIS, PL and QY measurements. Several parameters such as concentration, excitation wavelength and pH are studied. Zeta-potential analysis indicate that pH-induced (de-)protonation processes of functional moieties directly affect the n-π* energy bands. This results in unique pH-dependent absorption and emission characteristics which are discussed on the specific chemical composition of each CD system.
Extensometer sind seit Jahrzehnten im Einsatz und bilden die Basis für eine präzise Dehnungsmessung in werkstoffmechanischen Versuchen. Jedoch ist die Temperaturstabilität von Extensometern häufig noch nicht ausreichend beachtet worden, um Fehler verursacht durch Temperaturschwankungen zu minimieren. Dieses wird derzeit nicht nur in Deutschland, sondern auch international zunehmend diskutiert. Datenblätter von Extensometern sind teils unvollständig besonders hinsichtlich von Temperatureinflüssen. Extensometer für den Einsatz bei höheren Temperaturen sollen z.B. laut Normen für dehnungsgeregelte Ermüdungsversuche mit Luft oder Wasser aktiv gekühlt werden. Jedoch schreiben die Normen keine Temperatur-Toleranzen für Extensometer vor. Dehnungsfehler verursacht durch Temperaturschwankungen am Extensometer bleiben meist verborgen, da die Temperatur des Extensometers standardmäßig gar nicht gemessen wird. Die Ursache von Einflüssen zur Temperaturstabilität von Extensometern wird erläutert. Ein einfaches Rechenbeispiel zeigt die Empfindlichkeit von Extensometern gegenüber Temperaturschwankungen und die Auswirkungen auf den Dehnungsfehler. Lösungsmöglichkeiten zur Optimierung werden aufgezeigt. Der Anwender von Extensometern soll sensibilisiert werden, um der Temperaturstabilität von Extensometern sowohl hinsichtlich Herstellerspezifikationen als auch bei der Anwendung von Extensometern im Prüflabor mehr Aufmerksamkeit zu schenken, um letztlich die Qualität von Versuchsergebnissen zu verbessern. Empfehlungen an Extensometerhersteller werden formuliert. Dieses Thema wird zukünftig auch in Prüfnormen mehr Aufmerksamkeit geschenkt werden. Es werden Maßnahmen zur Verbesserung der Temperaturstabilität von Extensometern Einzug in Prüfnomen finden, um letztlich verlässlichere Versuchsergebnisse zu erhalten. Es ist beabsichtigt, eine Verbesserung der Temperaturstabilität von Extensometern z.B. bei der nächsten Revision der Prüfnormen ISO 12106 und ISO 12111 für dehnungsgeregelte LCF- und TMF-Versuche zu berücksichtigen.
Localized laser surface treatments are able to produce tailor-made surface properties to fulfill requirements of a variety of technical applications. Especially micrometric surface topologies can be beneficial for optimizing tribological contact situations. Structures with lowered surface features are already utilized for bearings or cylinders of combustion engines. There are also other fields of application, where the potential of protruding surface features is known, e. g. for metal forming tools.
A promising approach for a tailored surface treatment working in the microsecond range is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This technique is able to produce micrometric surface structures and to improve simultaneously the wear resistance by creating metal matrix composites.
In this talk, the laser implantation technique is described and compared to the state of the art. The potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces is demonstrated by means of microstructural and topographical investigations of different ceramic materials and steel substrates. Finally, results of research projects are presented aiming on the application of such structured surfaces. Their capability to change and optimize friction and wear are demonstrated for fully lubricated contacts, tools for hot sheet metal forming and tools for cold rolling of sheets for automotive applications.
Das Prozessmonitoring stellt einen wichtigen Baustein für eine Qualitätssicherung additiv gefertigter Bauteile dar, insbesondere bei kleinen Losgrößen. Der Vortrag zeigt einen Überblick aktueller Entwicklungen der BAM im Bereich des Prozessmonitorings für das Laserstrahlschmelzen (laser powder bed fusion) metallischer Werkstoffe. Durch Vergleich mit der Referenzmethode Computertomografie wird am Beispiel der thermografischen Verfahren gezeigt, wie relevante Defekte in Bauteilen detektiert werden können und Einsatzpotenziale sowie Limitierungen aufgezeigt.
Polymers of intrinsic microporosity (PIMs) have recently emerged as novel materials for a broad range of high-performance applications from gas separation to electronic devices. The very rigid, contorted polymer chains show only limited molecular mobility and therefore pack inefficiently giving rise to intrinsic microporosity with pore sizes generally smaller than 1 nm resulting in BET surface areas larger than 700 m2/g. Using conventional thermal analysis techniques, no glass transition temperature (Tg) of PIMs could be unambiguously detected up to now. Employing fast scanning calorimetry (FSC) based on a one chip sensor, decoupling the time scales responsible for the glass transition and the thermal decomposition is a reliable strategy to overcome this limitation. The FSC device is capable to heat and cool a small sample (ng-range) with ultrafast rates of several ten thousand K/s. Evidence of a glass transition is obtained for a series of PIMs with different chain rigidities. Local small-scale fluctuations are held responsible for the glass transition of highly rigid PIMs rather than segmental motions as in conventional polymers.
In diesem Verbundvorhaben werden standardisierte Messverfahren für hybride Gemische erarbeitet, die der Bestimmung sicherheitstechnischer Kenngrößen des Explosionsschutzes dienen. Unter einem hybriden Gemisch wird dabei ein mehrphasiges System aus Brenngas oder brennbarem Dampf, sowie Luft und brennbarem Staub verstanden. Die Veröffentlichung der Ergebnisse erfolgt in einem Abschlussbericht und als DIN-Spezifikation (DIN SPEC). Diese DIN SPEC versetzt Prüfinstitute und Industrie in die Lage, Explosionsgefahren beim Betrieb technischer Anlagen mit hybriden Gemischen einzuschätzen und damit Prozesse sowohl sicherer als auch effizienter zu steuern. Dieses Projekt wird im Rahmen des WIPANOProgramms (Wissens- und Technologietransfer durch Patente und Normen) vom BMWi gefördert.
Demonstrationsexperimente
(2019)
Korrosionsprüfung
(2019)
Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)-
Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement.
The European Commission's recommendation on the definition of nanomaterial [2011/696/EU] is broadly applicable across different regulatory sectors and requires the quantitative size Determination of constituent particles in samples down to 1 nm. A material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The implementation of the definition in a regulatory context challenges measurement methods to reliably identify nanomaterials and ideally also nonnanomaterials as substance or product ingredient as well as in various matrices.
The EU FP7 NanoDefine project [www.nanodefine.eu] addressed these challenges by developing a robust, readily implementable and cost-effective measurement strategy to decide for the widest possible range of materials whether it is a nanomaterial or not. It is based on existing and emerging particle measurement techniques evaluated against harmonized, material-dependent performance criteria and by intra- and inter-lab comparisons. Procedures were established to reliably measure the size of particles within 1-100 nm, and beyond, taking into account different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics.
A main outcome is the establishment of an integrated tiered approach including rapid screening (Tier 1) and confirmatory methods (tier 2), a decision support flow scheme and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool which implements the flow scheme in a user-friendly software and guides the user in a semi-automated way through the entire decision procedure. It allows a cost-effective selection of appropriate methods for material classification according to the EC's nanomaterial definition and provides a comprehensive report with extensive explanation of all decision steps to arrive at a transparent identification of nanomaterials as well as non-nanomaterials for regulatory
purposes.
As one of the widely used analytical methods for the analysis of elemental composition of solid matter, energy dispersive X-ray spectroscopy (EDS) has recently gained significant importance regarding its application to the chemical analysis of nanoparticles, especially in conjunction with the use of a scanning electron microscope (SEM) and the use of the transmission operation mode of SEM (STEM-in-SEM). This development was mainly driven by the technological progress with highly sensitive EDS detectors, such that individual nanoparticles can be quickly inspected with EDS at a SEM. Qualitative information on elemental composition with about 10 nm spatial resolution can be achieved complementary to the high-resolution information of the sample surface morphology within the same scanned area as provided by the electron microscope. Representative examples with successful EDS analysis on nanoparticles are presented, but also limitations of the method are described.
Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with Errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs.
An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal, has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. In the TEM micrograph the particles tracked manually according to the measurement protocol. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy.