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Eingeladener Vortrag
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Alkali and alkaline earth chlorides are discussed as heat storage media and are characterized by their low price and high availability. Disadvantages are a high corrosion rate and formation of Cr6+ ions in the melt, as observed in various binary chlorine salt melts. In our work the system NaCl-KCl-MgCl2 is considered. The storage capacity in this salt system is between 2 and 3 MWh per 10 t salt, depending on composition, melting temperature and working temperature. At the same time the system offers a eutectic line, which allows a high variance of the composition and possibly different corrosion rates can be observed. Corrosion tests in melts were carried out and the corrosion layers investigated. The tests with chloride melts on 12% Cr steel show an inner corrosion zone of up to 40 µm depth after 96 hours. The corrosion mechanisms and potential solutions are discussed.
Thermodynamic study of a refractory complex concentrated alloy (rCCA) using the CALPHAD method
(2019)
Multi-principal-element alloys (MPEAs), have recently come to the attention of the scientific community due to their potential for improving properties such as, e.g. mechanical strength and oxidation resistance in high temperature structural applications. The AlMo0.5NbTa0.5TiZr refractory (r)CCA is one such candidate, showing a two-phase microstructure after a two-stage heat treatment under argon atmosphere at a controlled cooling rate. Since the application conditions intended for this alloy require a long-term high temperature (> 700 °C) mechanical and oxidation resistance, it becomes necessary to assess the possible phase development in this regime. The diagrams reveal that two BCC-based phases could form during alloy solidification, where one phase would be enriched with Mo, Nb and Ta while the other phase, with Al, Ti and Zr. Activity oxides diagrams show that a stable form of aluminum oxide (α-Al2O3, Pearson symbol: hR10, corundum) can be formed.
Inorganic nanoparticles are used to improve the performance of epoxy as the matrix phase in fiber-reinforced composites used for aerospace applications. The effectiveness of nanofillers on property enhancement of thermosetting polymers depends on many factors including the interaction between the functional groups of nanofillers and the polymer reactants. In the current work, we study the effect of boehmite nanoparticles (BNPs) on properties of anhydride-cured bisphenol-A-diglycidyl ether (DGEBA). Dynamic mechanical thermal analysis (DMTA) and a high-resolution force measurement approach called intermodulation atomic force microscopy (ImAFM) were carried out to investigate the thermomechanical and nanomechanical properties of this material, respectively. It was found that BNPs lead to decrease of glass transition temperature (Tg) and crosslink density of the polymer network meanwhile significantly enhancing the Young’s modulus. Besides formation of a soft interphase near the particles, significant changes in local stiffness of polymer matrix far from the interphase was observed with ImAFM. Thus, boehmite induces long-range chemical alteration on the matrix. This effect has a higher impact on overall composite properties compared to the formation of interphase which is only a short-range effect. The local chemical evaluations on the soft interphase using an infrared-AFM method (NanoIR) revealed the accumulation of anhydride hardener near the boehmite interface. Based on these observations the effect of boehmite on the curing of epoxy is hypothesized to be governed by the strong interaction between boehmite and the anhydride. This interaction causes changes the ratio of reactants in the epoxy mixture and hence alteration of curing pathway and the network architecture. In future studies we examine this hypothesis by measuring the thermomechanical properties of cured epoxies in which the epoxy-hardener ratio is systematically altered and further comparing to those properties of nanocomposites shown in the current study.
The application of inorganic nanoparticles as reinforcement agent for polymer composites is constantly growing. Improving the performance of the material with desirable properties requires understanding of the interaction between polymer chains and nanoparticles and the properties of the interphase as well. Boehmite, a mineral of aluminum with basic unit of AlO(OH), is a novel and promising nanofiller which leads to enhanced performance of polymer composites. It has been recently reported that boehmite nanoparticles have reinforcing effect on epoxy matrix in carbon-fiber composites. It was primarily assumed that these improvements are due to very high Young’s modulus of boehmite particles. However, in our latest study we presented new values for the Young’s modulus of boehmite much lower than those reported earlier. This brings up the importance of interphase properties, e.g. the crosslink density, which can have the dominant role in the overall material property. Nevertheless, due to resolution limitations of conventional nanoprobing approaches, characterization of the interphase between individual particles and matrix is a challenge.
In this study, the main goal is to investigate the interphase of the epoxy/boehmite nanocomposites using AFM-based methods. We simplify the three-dimensional nanocomposite system to a two-dimensional horizontally layered sample with a large and easy to access interphase area. For this purpose, 1µm coatings of hydrothermally synthesized boehmite are prepared as the substrate on which the epoxy is later molded and cured. AFM surface potential and force maps were obtained on the cross-sectional cut of epoxy/ boehmite sample. The results show unexpectedly a large interphase area (approx. 1 µm) with different electrical and mechanical properties comparing to bulk epoxy. The average force-distance curves from this region showed more elastic behavior compared to bulk. The underlying mechanism of this influence is not fully understood yet. Thus, further investigation on the interphase region using the novel Nano-IR approach provides more information about the chemical characteristics. Numerical simulation will give complementary information to understand the effect of nanoparticles on the crosslinking density of the interphase. This can be different to bulk epoxy due to either different local temperature gradients or due to a surface selectivity of boehmite towards the monomer molecules.
Boehmite nanoparticles (AlOOH) were recently found to improve properties such as crack resistance, shrinkage and compressive strength in epoxy composites. Concentration and surface modification of boehmite nanoparticles are key factors for abovementioned enhancements. To understand the underlying mechanisms, more detailed research of micro- and nanoscopic mechanical properties is required. The presented study aims to investigate the influence of concentration and surface modification of boehmite on the stiffness of the bulk epoxy by means of AFM-based approaches: Force-Distance curves (FDC) on the sub- microscale and Intermodulation AFM and amplitude-dependent force spectroscopy (ADFS) on the nanoscale. For this purpose, stiffness-maps of epoxy filled with boehmite, with and without surface modification (HAc-boehmite) were obtained by FDC. These measurements showed a slight increase in overall stiffness of composite with increasing the nanoparticle content. The stiffening effect was observed to be intensified with HAc-boehmite. Since the lateral resolution of FDC is not high enough to distinguish nanoparticles, this effect was assumed to be due to the inevitable inclusion of nanoparticles in the measurement. By using Intermodulation-AFM, yielding ADFS stiffness maps with the resolution of <10 nm, we were able to calculate the average stiffness of bulk epoxy without the interference of nanoparticles. It was expected that the stiffness of regions faraway from particles would be equal to neat epoxy. In contrast, the results showed a drastic increase in stiffness of epoxy with increasing boehmite concentration (0, 1, 2.5, and 15%) especially in case of introducing 15wt% HAc-boehmite. Another important observation was formation of a spatial structure with non-homogenous stiffness distribution in bulk epoxy with HAc-boehmite. The underlying mechanisms of described observations are not fully understood yet. One hypothesis is the local increase in crosslinking density which we aim to investigate in our further studies by combining Dynamic Mechanical Thermal Analysis (DMTA) and Intermodulation-AFM.
THz and mid IR spectroscopy of high-molecular PE (HMW) and ultra high-molecular PE (UHMW) reveals modifications of the molecular structure. Characteristic absorption bands are changed if the two materials are exposed by γ-Co60 radiation up to 600 kGy and subsequently stored at an annealing temperature of 398 K until for 729 days. UHMW-PE and HMW-PE behave differently during the ageing process because of their molecular weight and inherent structure distinctions. The spectroscopic data offer characteristic absorption bands, which have been used to describe the complete ageing process in more detail. For instance, the integral absorption in the B1u THz-region can be used to describe quantitatively the reduction of crystallinity. The formation of trans vinylene unsaturation and the decay of vinyl during ageing can be observed in detail in the mid IR range.
Morphologies of Fresnoite surface crystals of BT0.75S glass under different atmospheric conditions
(2019)
Fresnoite glass-ceramics are characterized by piezoelectric, pyroelectric and non-linear optical properties. These properties can be adjusted by orienting the fresnoite crystals during crystallization. Crystallization begins at the surface. The first surface crystals are not oriented perpendicular and, therfore, produce a surface layer that has not the intended properties. To overcome this issue, the formation of fresnoite surface crystals at different atmospheric conditions was studied.
Synchrotron based absorption edge tomography for the analysis of 3D printed polymer embedded MOF
(2019)
Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well.
In this work, metal organic frameworks (MOFs) embedded in polymer are characterized using differential tomography. MOFs are microporous structures of metal ions, coordinated by organic linker molecules, that can be used in a broad field of applications, especially in gas storage and catalysis. In this work, polymer embedded MOFs were extruded into filaments, which were subsequently used for 3d-printing to profit from the specific properties of the MOFs in polymeric materials combined with the arbitrary shapes provided by 3d-printing. For the extrusion, different polymer classes like ABS, polyester- and polyetherurethanes, as well as different MOFs (ZIF-8, ZIF-67, HKUST-1) were used to create MOF containing filaments with a nominal diameter of 3.0 mm. Differential tomography at the edges of the Zn, Co, and Cu was then used to find the distribution of the corresponding MOF in the filament and to analyze the shape of the inclusions.
Die Porosität sowie die Porengrößenverteilung (PSD) eines Baustoffs sind wichtige petrophysikalische Eigenschaften, die Transportprozesse im Material beeinflussen und im direkten Zusammenhang mit der Schadensanfälligkeit stehen (Frost-Tau-Schäden, Schäden durch Salzeinträge und sauren Regen). Verfahren zur Ermittlung der Porosität stellen die Quecksilberporosimetrie (MIP), das Prinzip der Tauchwägung nach Archimedes (triple weighing method, TWM) und die Nuklear Magnetische Resonanz (NMR) dar.
Das Hauptziel dieser Arbeit ist der Vergleich der drei Methoden für die Porositätsbestimmung. Als Untersuchungsmaterial wurde Sandstein gewählt. Als Baustoff wird Sandstein trotz einer teilweise geringen Festigkeit, aber aufgrund seiner Farbvielfalt häufig für Kulturbauten, Gehwegmaterial und Fassaden eingesetzt. Sandsteine weisen zudem meist eine hohe effektive Porosität (bis zu ca. 30 %) und teilweise breite Porengrößenspektren auf, wodurch Feuchte- und Ioneneinträge begünstigt werden und zu z. B. langfristigen Verfärbungen an Sandsteinfassaden führen können.
Im Rahmen dieser Arbeit werden die Porositäten von 10 verschiedenen Sandsteinen aus Deutschland und Tschechien bestimmt. Für die Untersuchungen mittels TWM und NMR wurden für jede Sandsteinart zwei zylinderförmige Proben unter Unterdruck mit Leitungswasser aufgesättigt. Beim Vergleich der Verfahren liegt der Fokus insbesondere auf NMR und der verwendeten Gerätetechnik, die mit einer minimalen Echozeit von 50 µs ein Wasserstoffsignal in Sandsteinen aus bis zu ca. 2 nm kleine Poren erfassen kann. Darüber hinaus wird das Auflösungsvermögen von MIP und NMR bezüglich der Poren- bzw. Poreneingangsgrößen diskutiert. Für den Vergleich von NMR und MIP werden an ausgewählten Sandsteinproben ebenfalls die zusätzlich ermittelten PSD in Korrelation zueinander gebracht.
Erste Ergebnisse zeigen eine gute Korrelation von NMR- und TWM-Daten, aber teilweise starke Abweichungen zu den mit MIP bestimmten Porositäten. Ergebnisse zu den PSD zeigen teilweise nahezu identische Kurvenverläufe. Jedoch ist die Abschätzung des Umrechnungsfaktors für die NMR-Daten ohne Hinzuziehen von zusätzlichen Referenzverfahren wie Röntgen-Computer-Tomographie oder Spektral Induzierte Polarisation teilweise sehr schwierig.
Extracellular vesicles (EV) are cell-derived particles in body fluids, which have excellent potential as next-generation biomarkers. The exploitation of EV requires reliable measurements, which is currently very difficult, as most EV are smaller than 200 nm. At present, flow cytometry (FCM) is the most appropriate technique for EV analysis in biological samples, as FCM is readily available in many clinical laboratories and allows to identify cell-specific EV at high throughput. However, due to technical variations between different FCM instruments, EV concentration measurements are currently not well comparable between most laboratories. Therefore, EV reference materials and standardized reference methods are urgently needed to calibrate flow rate, light scattering intensity, and fluorescence intensity of FCM in the sub-micrometer size range. This requires a better matching of the optical properties of calibration beads and EV as can be realized with current polystyrene calibration beads.
The EMPIR project 18HLT01 “MetVes II” aims to develop synthetic reference materials and traceable measurement methods to standardize EV measurements. The reference materials should resemble EV properties, so that calibrations are reliable and do not require a change of acquisition settings. Hence, the reference materials should contain particles with a traceable number concentration in the range of 109–1012 particles/mL to calibrate flow rate, a traceable size with discrete diameters between 50–1000 nm and a refractive index (RI) in the range of 1.37–1.42 to calibrate scattering intensity, and a traceable fluorescence intensity between 100–100,000 molecules of equivalent soluble fluorochromes (MESF). At BAM, various approaches to prepare such low-RI nanometer-sized reference materials will be studied, preliminary results of the primary characterization of these candidate reference particles will be presented, and possible applications besides FCM-based EV detection will be outlined.
Metal phosphonates are promising materials for applications in fuel cells, due to their high proton conductivity and higher chemical and thermal stability compared to the industry standard (e.g. Nafion®). Additionally, metal phosphonates are precursors to porous carbon materials with evenly distributed centers for ORR catalysis. As a fast and sustainable synthesis, mechanochemistry is the synthesis method of choice. Thorough characterization is carried out by XRD, MAS-NMR, XAS, BET, and DVS.
Nanoparticles (NPs) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications.
Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles.
Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni.
Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage.
We present the synthesis of monodisperse monometallic Ni nanoparticles (NPs) and bimetallic NiCu respectively NiCo NPs. The NPs were investigated using SAXS, STEM, EDX, and XANES, showing that the NPs are size tunable and stable while the surface is not entirely covered. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4.
Nanoparticles (NP) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications.
Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles.
Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni.
Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage.
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks [1-2]. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink [3] and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [4]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
[1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004
[2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013
[3] S. Centeno, J. Shamir Journal of Molecular Structure, 873 (2008), 149-159
[4] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
First, we will provide an overview of the sources [1-2] employed in the study – dating from 9th to 14th century, although the manuscripts in which they can be found dates up to the 20th century – with an eye on the ink typologies (real and perceived by the compilers). Then we will show how, by reproducing the recipes, it was possible to shed light on some oddities in the procedures and the choice of ingredients. In the end we will discuss problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [3]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol and the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
[1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004
[2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013
[3] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50
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.
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.