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- Korrosionsschnelltest (6)
- NIR (6)
Structural health monitoring contributes to early damage detection in the built infrastructure. During the last two decades, sensor networks transferred from wired to wireless sensor networks. Several methods exist to measure moisture in building materials. Most of the introduced commercial moisture measurement methods provide information about the local or near surface moisture. A feasibility study is presented to demonstrate, how the Received Signal Strength Indicator (RSSI) of a Bluetooth Low Energy (BLE) signal, transmitted from the BLE-module embedded in building materials, correlate with changing moisture content. The feasibility of this influence was investigated in the presented study. The maximum and minimum RSSI were systematically recorded and analysed.
Particle size gradation is regarded as an effective method for overcoming the contradicting requirements in three-dimensional printing (3DP). In present work, particle size gradation was optimized to obtain both acceptable flowability of the powder material and high-strength 3D-printed glass-ceramic products. The effect of gradation on the printing process, sintering process and performance of the 3D-printed glass-ceramic products was investigated comprehensively. The glass-ceramic powders with three size ranges were mixed in certain proportions and applied to print parts. The result showed parts printed with powder mixed by 60 wt% 45–100 µm and 40 wt% 0–25 µm particles had satisfactory density of 1.60 g/cm³ and bending strength of 13.8 MPa. The flowability decreased with an increasing proportion of fine particles. Part density was determined by the powder bulk density in the powder bed as well as the shrinkage during sintering while strength of part was found to be dependent on the sintering degree.
Nanocomposites of Ag-ZnFe2O4@reduced graphene oxide (rGO) were synthesized using a one-pot microwave-assisted self-assembly method. The morphology and structure of the Ag-ZnFe2O4@rGO nanocomposites were characterized. The nanocomposites formed with 15.2 wt% rGO showed excellent adsorption properties and high photocatalytic activity for the degradation of methylene blue (MB), rhodamine B (RhB), and methyl orange (MO). The synergistic interactions between Ag, ZnFe2O4, and rGO decreased the aggregation of the nanoparticles (NPs) and increased the surface area, resulting in better absorption in both UV and visible light. Such a structure was helpful for separating the photoexcited electron-hole pairs and accelerating electron transfer. Electrochemical impedance spectroscopy (EIS) revealed a smaller resistance in the solid-state interface layer and charge transfer on the composite surface than that of the bare ZnFe2O4 NPs and ZnFe2O4@rGO nanocomposite. The Ag-ZnFe2O4@rGO nanocomposite could be recovered easily by a magnet and reused five times with no significant decrease in photocatalytic activity. The as-prepared Ag-ZnFe2O4@rGO nanocomposite catalyst could be applied to the removal of hard-to-degrade waste materials owing to its high efficiency in both UV and visible light and its excellent reusability.
If fracture mechanics shall be applied to the total lifetime respectively the fatigue limit of components (within the meaning of the S-N curve approach) it has to address four challenges:
(a) It has to adequately describe so-called short crack propagation, which cannot be based on the common long crack concepts for principle reasons. Since the crack size is in the order of the plastic zone size, the modelling of short crack propagation cannot be based on the common linear elastic Delta K concept. Instead, an elastic-plastic parameter such as the cyclic J integral has to be applied. A second point is that the crack closure concept has to be modified in that the crack opening stress is not a constant, crack size- independent parameter but shows a transient behaviour with increasing short crack size.
(b) It has to provide a meaningful definition of the initial crack dimensions as the starting point for an S-N curve relevant (residual) lifetime analysis. This can be based either on the (statistical) size of material defects which can be treated as cracks or by the size of the crack which would arrest subsequent to early crack propagation, whatever is larger.
(c) It has to cope with the problem of multiple cracks for load levels higher than the fatigue limit such as it occurs in many applications in the absence of very large initial defects.
(d) This requires consequent statistical treatment taking into account variations in the local geometry of the area where crack initiation has to be expected as well as the scatter in the initial crack size and in the material data used for the analyses.
The paper provides an overview on the results of a German cluster project on the use of fracture mechanics to the determination of the fatigue strength of weldments with fatigue cracks originating at the weld toes. The approach includes (a) a concept for short crack propagation for which the common ΔK concept is not applicable and the crack closure effects are still being gradually build-up, (b) a method for determining fatigue life relevant initial crack sizes as they are needed in any fracture mechanics analysis and (c) multiple cracking and crack coalescence at load levels higher than the endurance limit. The analyses are stochastically performed. Both, the endurance limit and the finite life branch of the S-N curve are determined.
Besides a brief introduction into the approach, validation examples are presented. These comprise different weldment types (butt welds, cross joints and longitudinal stiffened plates), two steels (S355NL and S960QL) of quite different strengths, different weld geometries due to different welding techniques (WIG, MAG), as-welded and stress relieved welds and different stress ratios varying from R = -1 to R = 0.5.
Rohrsysteme und Behälter aus nichtrostendem Stahl sind mit einer Passivschicht vor Korrosion geschützt. Ist diese jedoch unvollständig ausgebildet oder beschädigt, geht der Schutz verloren. Das KorroPad-Verfahren ist ein Schnelltest zur Überprüfung der Passivschicht. Im Vergleich mit bisher üblichen Bewertungsmethoden ist die Anwendung sehr einfach und nimmt nur 15 Minuten in Anspruch.
Miniaturized pacemakers with a surface consisting of a Ti alloy may have to be removed after several years from their implantation site in the heart and shall, therefore, not be completely overgrown by cells or tissue. A method to avoid this may be to create at the surface by laser-ablation self-organized sharp conical spikes, which provide too little surface for cells (i.e., fibroblasts) to grow on. For this purpose, Ti-alloy substrates were irradiated in the air by 790 nm Ti:sapphire femtosecond laser pulses at fluences above the ablation threshold. The laser irradiation resulted in pronounced microstructure formation with hierarchical surface morphologies. Murine fibroblasts were seeded onto the laser-patterned surface and the coverage by cells was evaluated after 3–21 days of cultivation by means of scanning electron microscopy. Compared to flat surfaces, the cell density on the microstructures was significantly lower, the coverage was incomplete, and the cells had a clearly different morphology. The best results regarding suppression of cell growth were obtained on spike structures which were additionally electrochemically oxidized under acidic conditions. Cell cultivation with additional shear stress could reduce further the number of adherent cells.
Titanium nitride (TiN) was coated on different substrate materials, namely pure titanium (Ti), titanium alloy (Ti6Al4V) and steel (100Cr6), generating 2.5 μm thick TiN layers. Using femtosecond laser pulses (30 fs, 790 nm, 1 kHz pulse repetition rate), large surface areas (5 mm × 5 mm) of laser-induced periodic surface structures (LIPSS) with sub-wavelength periods ranging between 470 nm and 600 nm were generated and characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). In tribological tests, coefficients of friction (COF) of the nanostructured surfaces were determined under reciprocating sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel during 1000 cycles using two different lubricants, namely paraffin oil and engine oil. It turned out that the substrate material, the laser fluence and the lubricant are crucial for the tribological performance. However, friction and wear could not be significantly reduced by LIPSS on TiN layers in comparison to unstructured TiN surfaces. Finally, the resulting wear tracks on the nanostructured surfaces were investigated with respect to their morphology (OM, SEM), depth (WLIM) and chemical composition by energy dispersive X-ray spectroscopy (EDX) and, on one hand, compared with each other, on the other hand, with non-structured TiN surfaces.
The presentation will discuss the difference between EU and US standards for the determination of explosion (flammability) limits and limiting oxygen concentration. Small differences observed in measured values can be traced back to the different test apparatuses and criteria. The discrepancies can be much greater in the case of limiting oxygen concentration because of the high amount of inert gases and the corresponding low laminar burning velocities. The paper describes some examples and the influence of the chosen criteria on the results. The European and US standards use the criteria of flame propagation in open test vessels and of pressure rise in closed ones. The examples discussed show that flame propagation is still possible at very small pressure rise values, as observed much below the pressure rise criterion of usual standards. However, flame propagation in a process plant can cause an accident or explosion and must be avoided. Therefore, the flame propagation criterion is recommended to be used in chemical safety engineering. The European safety database CHEMSAFE contains expertevaluated safety data for cases where the determination method and criteria are known. Flammability characteristics based on the pressure rise criterion may suffice in certain cases, e.g. for explosion protection in closed vessels without any connecting pipes.
Force-distance curves have been acquired with an atomic force microscope on perfluorpolyether films. It is shown that curves acquired on films of different thickness, at different rates and with different dwell times can be overlapped by rescaling the time or distance axis.When the time or distance axis is rescaled,the force depends only on the surface tension of perfluorpolyether and on geometrical properties of thetip (aperture and perimeter of the tip at a given distance from the apex). Hence, curves acquired with thesame tip overlap.
By comparing curves acquired at different rates the dynamics of tip-wetting can be investigated. Fur-thermore, rescaled force-distance curves have been matched with the perimeter of cross sections ofthe tip, i.e. with the perimeter of the three-phase contact line. Such measurements pave the way for anon-destructive investigation of the tip shape.
Artificial light harvesting complexes find applications in artificial photosynthesis, photovoltaics and light harvesting chemical sensors. They are used to enhance the absorption of light of a reaction center which is often represented by a single acceptor. Here, we present different light harvesting systems on DNA origami structures and analyze systematically the light harvesting efficiency. By changing the number and arrangement of different fluorophores (FAM as donor, Cy3 as transmitter and Cy5 as acceptor molecules) the light harvesting efficiency is optimized to create a broadband absorption and to improve the antenna effect 1 (including two energy transfer steps) from 0.02 to 1.58, and the antenna effect 2 (including a single energy transfer step) from 0.04 to 8.7, i.e. the fluorescence emission of the acceptor is significantly higher when the light-harvesting antenna is excited at lower wavelength compared to direct excitation of the acceptor. The channeling of photo energy to the acceptor proceeds by Förster Resonance Energy Transfer (FRET) and we carefully analyze also the FRET efficiency of the different light harvesting systems. Accordingly, the antenna effect can be tuned by modifying the stoichiometry of donor, transmitter and acceptor dyes, whereas the FRET efficiency is mainly governed by the spectroscopic properties of dyes and their distances.
The damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC), relevant for PE-HD materials are characterized based on improved full notch creep testing (FNCT) of two selected typical PE-HD materials for container applications. In this context, a distinction of the failure mechanisms as well as a categorization of involved media is suggested. Employing a novel FNCT device, elongation data were obtained in addition to conventional time-to-failure results of stress-dependent as well as temperature-dependent measurements. Changes in failure behavior, as determined by fracture surface analysis based on light microscopy (LM) and laser scanning microscopy (LSM), are correlated with FNCT results and used to introduce an additional possibility for the identification of brittle/ductile fracture behavior.
Nanolenses are self-similar chains of metal nanoparticles, which can theoretically provide extremely high field enhancements. Yet, the complex structure renders their synthesis challenging and has hampered closer analyses so far. Here, DNA origami is used to self-assemble 10, 20, and 60 nm gold nanoparticles as plasmonic gold nanolenses (AuNLs) in solution and in billions of copies. Three different geometrical arrangements are assembled, and for each of the three designs, surface-enhanced Raman scattering (SERS) capabilities of single AuNLs are assessed. For the design which shows the best properties, SERS signals from the two different internal gaps are compared by selectively placing probe dyes. The highest Raman enhancement is found for the gap between the small and medium nanoparticle, which is indicative of a cascaded field enhancement.
High temperature oxidation of 9–12% Cr ferritic/martensitic steels under dual-environment conditions
(2017)
In normal operations, the opposite surfaces of the power plant components are exposed to two different environments, i.e. air/flue gas on the one side and steam on the other side. Exposure under such dual-environment can lead to accelerated corrosion of the components on the air side. The oxidation behaviour of ferritic/martensitic steel T92 was investigated under dual-environment in a specially designed test equipment. The samples were exposed to dry oxyfuel flue gas (CO2–27%N2–2%O2–1%SO2) on one side and to steam on the other side up to 1000 h at 650°C. The formation of oxide scales was characterised by optical microscopy and scanning electron microscopy with attached energy-dispersive spectroscopy. Oxidation rate of specimens under dual-Environment condition was almost three times higher than that in single-environment condition. This is explained based on hydrogen transport through the bulk alloy from the steam side to the flue gas side.
The aim of the present work was to investigate the possibilities of hybrid laser arc welding regarding reliable production of longitudinal welds of high strength pipe steels X80 and X120 and to evaluate achievable mechanical properties of laser hybrid welds. The study focused on weld toughness examination in low temperature range up to -60 °C. SЮТЭКЛХО ПТХХОЫ ЦКЭОЫТКХЬ were identified in the context of this task. It could be shown that metal cored electrodes guaranteed sufficient Charpy impact toughness at low temperature for both investigated materials. Modern arc welding technologies such as modified pulsed spray arc were used to promote deeper Penetration of the filler material into the narrow laser welding gap. Edge preparation with a 14 mm deep root face was considered as optimum, because no penetration of the filler material could be detected beyond this depth limit and therefore any metallurgical influences on the weld metal properties through the welding wire could be excluded.
Efficient water oxidation catalysts are required for the development of water splitting technologies. Herein, the synthesis of layered hybrid NiFephenylphosphonate compounds from metal acetylacetonate precursors and phenylphosphonic acid in benzyl alcohol, and their Oxygen evolution reaction performance in alkaline medium, are reported. The hybrid particles are formed by inorganic layers of NiO6 and FeO6 distorted octahedra separated by bilayers of the organic group, and template the Formation in situ of NiFe hydroxide nanosheets of sizes between 5 and 25 nm and thicknesses between 3 and 10 nm. X-ray absorption spectroscopy measurements suggest that the hybrid also acts as a template for the local structure of the metal sites in the active catalyst, which remain distorted after the transformation. Optimum electrocatalytic activity is achieved with the hybrid compound with a Fe content of 16%. The combination of the synergistic effect between Ni and Fe with the structural properties of the hybrid results in an efficient catalyst that generates a current density of 10 mA cm−2 at an overpotential of 240 mV, and also in a stable catalyst that operates continuously at low overpotentials for 160 h.
This paper describes austenitic-ferritic duplex stainless steels, SAF 2205, in the presence of hydrogen. The duplex stainless steels (DSS) properties include excellent resistance to stress corrosion cracking, high strength and good weldability. Those steels are preferably used in industries combining hydrogen and loads. Hydrogen location in addition to hydrogen binding energy with the steel's defects are of great importance for the analysis of hydrogen embrittlement model in that steel. It is known from previously published works that the susceptibility to hydrogen embrittlement will depend on the competition between reversible and irreversible traps; meaning a direct relation to the hydrogen's state and position in the steel. In this work, we examine the local hydrogen concentration, trapping and distribution by two modern and advanced techniques: thermal desorption spectrometry (TDS) and we support it by time of flight-secondary ion mass spectrometer (ToF-SIMS). In this paper, we support and give for the first time new insights and better understanding to the hydrogen embrittlement mechanism in SAF 2205. The trapping energies levels were calculated using TDS and Lee and Lee's model. This model revealed reversible in addition to irreversible trapping sites. Also the trapping controlling mechanism was found to be a combination of detrapping controlled mechanism and diffusion controlled mechanism. The use of ToF-SIMS for local imaging the distribution of hydrogen species supports the discussion of the different hydrogen traps in this type of steel. The hydrogen embrittlemet phenomenon in SAF 2205 will be discussed in details in that paper.
Hyperbranched poly(amidoamine)/kaolinite nanocomposites: Structure and charge carrier dynamics
(2017)
An ex-situ approach was applied to prepare nanocomposites from hyperbranched poly(amidoamine) and modified kaolinite (Ka-DCA). The structure of the polymer and the corresponding nanocomposites was investigated by FTIR, DSC, SAXS and TEM. SAXS might suggest a partly exfoliated structure of the nanocomposites, which was supported by TEM. The molecular dynamics was studied by means of broadband dielectric spectroscopy (BDS). The dielectric spectra are dominated by a conductivity
contribution at higher temperatures for all samples investigated. The obtained results further indicated that DC conductivity is increased by 4 orders of magnitude with increasing concentration of Ka-DCA nanofiller. Further, a significant separation between the conductivity relaxation time and that of segmental dynamics was observed. The decoupling phenomenon and the conductivity mechanism were discussed in detail. This study provides insights about the influence of the nanofiller on the structure and the conductivity contribution of nanocomposites of hyperbranched polymers including the decoupling phenomenon and fragility.
Aluminum has gathered toxicological Attention based on relevant human exposure and its suspected hazardous potential. Nanoparticles from food supplements or Food contact materials may reach the human gastrointestinal tract.
Here, we monitored the physicochemical fate of aluminum containing nanoparticles and aluminum ions when passaging an in vitro model of the human gastrointestinal tract. Smallangle X-ray scattering (SAXS), transmission electron microscopy (TEM), ion beam microscopy (IBM), secondary ion beam mass spectrometry (TOF-SIMS), and inductively coupled plasma mass spectrometry (ICP-MS) in the singleparticle mode were employed to characterize two aluminumcontaining nanomaterials with different particle core materials (Al0, γAl2O3) and soluble AlCl3. Particle size and shape remained unchanged in saliva, whereas strong Agglomeration of both aluminum nanoparticle species was observed at low pH in gastric fluid together with an increased ion release. The levels of free aluminum ions decreased in intestinal fluid and the particles deagglomerated, thus liberating primary particles again. Dissolution of nanoparticles was limited and substantial changes of their shape and size were not detected. The amounts of particle-associated phosphorus, chlorine, potassium, and calcium increased in intestinal fluid, as compared to nanoparticles in standard dispersion.
Interestingly, nanoparticles were found in the intestinal fluid after addition of ionic aluminum. We provide a comprehensive characterization of the fate of aluminum nanoparticles in simulated gastrointestinal fluids, demonstrating that orally ingested nanoparticles probably reach the intestinal epithelium. The balance between dissolution and de novo complex formation should be considered when evaluating nanotoxicological experiments.
Copper, magnetite and graphite particles were mixed in order to observe their impact on the coefficient of friction (CoF) during pin-on-disc tests and on the tribofilm formation after testing. Pure magnetite powder provided a value of CoF of 0.4. Magnetite-copper mixtures tested at 400 °C revealed lower CoF values (~0.4) than those at room temperature (~0.6). Magnetite-graphite and magnetite-graphite-copper mixtures presented lower CoF values (~0.3). All systems formed a magnetite-based tribofilm and patches of metallic copper were found on the tribosurfaces of the mixtures containing copper. Carbon layers and graphite nanoinclusions were observed in the graphite mixtures. The incorporation of zirconia particles, a by-product of ball milling mixing, prevented the selective transfer of graphite and copper to the tribosurfaces of some of the samples.
Implementation of Ba0.6Sr0.4TiO3-ZnO-B2O3 based tunable microwave phase shifters in LTCC technology
(2017)
Tunable dielectric Ba0.6Sr0.4TiO3-ZnO-B2O3 thick-films were analyzed regarding their integration potential into the LTCC technology. Therefore, tunable loaded line phase shifters based on metal-insulator-metal varactors with single- and double- printed BST thick-films were fabricated and co-sintered inside a four layer LTCC module. Microstructural and chemical investigations showed a sufficient compatibility and adhesion between the silver, BST composite and LTCC layers and a resulting morphology depending on the processing route. The microwave characterization of the LTCC-embedded phase shifters revealed comparable results to phase shifters with the same design on alumina substrates.
In situ EDXRD study of MAG-welding using LTT weld filler materials under structural restraint
(2017)
Welding using low transformation temperature (LTT) filler materials is an innovative approach to mitigate detrimental welding residual stresses without cost-intensive post weldtreatments. Due to the local Generation of compressive residual stresses in the weld line by means of a delayed martensite transformation a significant enhancement of the cold cracking resistance of highly stressed welded components can be expected. For the effective usage of These materials a deeper understanding of the microstructural evolution inside the weld material is necessary to determine the complex processes that cause the residual stress formation during welding. Solid-state phase transformation kinetics and the evolution of strain in LTT weld filler materials are monitored in-situ at the instrument ID15A at the ESRF in Grenoble, France. The transferability to real components is implemented by using a realistic MAG welding process under consideration of structural restraint. During welding of multilayer joints, the phase Transformation and phase specific strain evolution of each individual layer is investigated in transmission geometry by means of energy-dispersive X-ray diffraction EDXRD using high energy synchrotron Radiation with a counting rate of 2.5 Hz. The measurement results of a 10% Cr / 10% Ni LTT weld filler are compared to data monitored for the conventional weld filler material G89. The in-situ data clearly indicate a strong effect on the local strain evolution and the formation of compressive strain. This results from the restraint volume expansion during the postponed austenite to martensite transformation of the LTT weld filler, which counteracts the thermal shrinkage. In contrast, for the conventional weld filler material the thermal contraction strains lead to tensile residual strain during welding. Furthermore, the results of in-situ observation during welding Show that the transformation kinetic is dependent on the welding sequence.
Shrinkage measurements of miniaturized low temperature co-fired ceramics (LTCC) samples under load typically lead to collapsing of the samples, which hampers the characterization of shrinkage up to full densification. In this paper, a measurement setup is presented, which allows for in situ shrinkage measurements of practical, large LTCC panels during pressure-assisted sintering in a sintering press. The shrinkage behavior of two commercial LTCC systems (GreenTape 951 and Ceramtape GC) has been measured under loads of up to 1 MPa. No crushing of the specimens was observed and reproducible characterization of shrinkage up to full densification has been performed. Based on comparisons to thermomechanical analyzer measurements in this and other studies, it was found that the in situ approach is much better suited for shrinkage characterization of LTCC under load.
Reproducibility and accuracy of the method are discussed and practical as well as more academic applications are proposed.
Several cylindrical specimens and dental implants, presenting diagonal lattice structures with different cell sizes (600, 900 and 1200 µm) were additively manufactured by selective laser melting process. Then they were implanted for two months in a sheep. After removal, they were studied by Archimedes’ method as well as X-ray computed tomography in order to assess the penetration of bone into the lattice. We observed that the additive manufactured parts were geometrically conform to the theoretical specifications. However, several particles were left adhering to the surface of the lattice, thereby partly or entirely obstructing the cells. Nevertheless, bone penetration was clearly visible. We conclude that the 900 µm lattice cell size is more favourable to bone penetration than the 1200 µm lattice cell size, as the bone penetration is 84 % for 900 µm against 54 % for 1200 µm cell structures. The lower bone penetration value for the 1200 µm lattice cell could possibly be attributed to the short residence time in the sheep. Our results lead to the conclusion that lattice implants additively manufactured by selective laser melting enable better bone integration.
At BAM, which is the federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes the assessment of the service lifetime of elastomeric seals that are part of the container lid system with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) up to 1.5 years. In order to assess sealability, O-rings are aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings are aged as well. Further methods characterising seal performance are compression stress relaxation (CSR) reflecting the loss of sealing force of a compressed seal over time, and compression set (CS) which represents the recovery behaviour of a seal after release from compression. Additionally, hardness is measured for information about the change of mechanical properties. The experimental results indicate that while hardness, CSR and CS show considerable degradation effects, the leakage rate stays relatively constant or even decreases until shrinkage combined with the loss of resilience of the aged seal leads to leakage. This demonstrates that static leakage rate, which is the only available direct seal performance criterion, has only limited sensitivity towards the degradation of the seal material. CS data is extrapolated using time-temperature shifts and Arrhenius graphs. An exemplary CS of 50 % would be reached after approx. 1.2, 17 and 29 years at 60 °C for HNBR, EPDM and FKM respectively.
The fatigue behaviour of cast iron is usually investigated on machined specimens. Components of cast iron, however, have a casting skin; therefore the investigation of the influence of the casting skin on the lifetime is of interest. To study this influence isothermal fatigue tests were carried out on heat-resisting spheroidal graphite cast iron EN GJS SiMo 4.05 in 4–point-bending set-up at 400 °C. Specimens with and without casting skin were investigated comparatively. The number of cycles to failure was significantly lower for specimens with casting skin. Metallographic investigations underline the reduction of lifetime caused by casting skin.
A long list of criteria determining the hot cracking susceptibility already exists. A main influence on solidification cracking can result from the design of the welded construction, i.e. from the influence of external loads. Using the Controlled Tensile Weldability (CTW) test, an external load hot cracking test, the influence of constant pre-load and different extension rates on the solidification cracking behavior of GTA (Gas Tungsten Arc) welds in an austenitic (AISI 309) and a ferritic (AISI 441) steel were investigated. Compared to specimens welded allowing free shrinkage and welded with an applied constant tensile pre-load, the specimens welded during the application of increasing tensile load show solidification cracks. In the weld seams, a characteristic angle α between the predominantly columnar grains and the fusion line can be observed. Specimens showing solidification cracks show a significantly larger angle α compared to the crack-free specimens. Based on these observations, the characteristic angle α is proposed as a new hot cracking criterion.
Biofilm formation poses high risks in multiple industrial and medical settings. However, the robust nature of biofilms makes them also attractive for industrial applications where cell biocatalysts are increasingly in use. Since tailoring material properties that affect bacterial growth or its inhibition is gaining attention, here we focus on the effects of femtosecond laser produced nanostructures on bacterial adhesion. Large area periodic surface structures were generated on steel surfaces using 30-fs laser pulses at 790 nm wavelength. Two types of steel exhibiting a different corrosion resistance were used, i.e., a plain structural steel (corrodible) and a stainless steel (resistant to corrosion). Homogeneous fields of laser-induced periodic surface structures (LIPSS) were realized utilizing laser fluences close to the ablation threshold while scanning the sample under the focused laser beam in a multi-pulse regime. The nanostructures were characterized with optical and scanning electron microscopy. For each type of steel, more than ten identical samples were laser-processed. Subsequently, the samples were subjected to microbial adhesion tests. Bacteria of different shape and adhesion behavior (Escherichia coli and Staphylococcus aureus) were exposed to laser structures and to polished reference surfaces. Our results indicate that E. coli preferentially avoids adhesion to the LIPSS-covered areas, whereas S. aureus favors these areas for colonization.
A combined experimental and numerical approach is applied for a numerical analysis of the non-uniform martensitic transformation kinetic on welding residual stresses and distortion of a single pass weld. The (γ → α)-transformation kinetic within the weld pool region is governed by a non-uniform distribution of the elements chromium and nickel. The single-pass weld was performed by use of the low-alloyed high-strength steel S960QL with the high-alloyed high-strength filler wire CN 13/4-IG®. A thermo-mechanical FE model of the welding process was experimentally validated against temperature field, solid phase distribution, transformation behaviour, X-Ray stress measurements and transient optical distortion measurements.
The experimentally determined and calculated weld residual stresses and transient distortion are in good agreement. It can be shown that the change on the (γ → α)-transformation kinetic driven by the inhomogeneous distribution of the chemical contents causes a strong influence on the weld residual stresses within the volume of the weld pool, which could promote crack propagation within the solidified weld pool by use of high-alloyed filler materials. Furthermore, a significant influence on the development of the transient welding distortion is visible. This influence should be respected during numerically calculation of welding distortion in case of multi-pass welding using interpass temperatures and high-alloyed filler materials.
The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polished or blasting depending on the application and the requested corrosion resistance. Blasted surfaces are often used in industrial practice due to the easier and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the different performed corrosion tests (potential measurement, KorroPad-test and pitting potential) on welding seams with different surface treatments.
Influence of weathering on the leaching behaviour of zinc and PAH from synthetic sports surfaces
(2017)
Synthetic materials used for outdoor sports grounds consist of a mix of inorganic, organic and polymeric compounds that show ageing due to weathering and a complex leaching behaviour by percolation of rainwater, which can limit its lifetime. Additionally, weathering exposure induces degradation processes in the polymers, which leads to the formation of new surfaces allowing water to access additional reservoirs of leachable compounds. A laboratory test comprising artificial weathering, ozonisation and subsequent leaching was developed to investigate this behaviour in a reproducible and controllable way. The experiments showed a general decline of Zn, polycyclic aromatic hydrocarbons (PAH) and total organic carbon (TOC) concentrations after an initial increase. Within this general trend, the course of concentration over exposure duration is very specific for individual sample materials and the analyte under investigation. The results indicate that weathering and degradation behaviour cannot be predicted from initial material conditions. Thus, weathering experiments are recommended to fill this gap of knowledge.
Polysaccharides are incorporated into cement based Systems in order to modify the rheological properties. Typically, cellulose ethers, sphingan gums, guar gum or starch ethers are applied. Depending upon their chemistry, molecular architecture, and adsorption tendency, polysaccharides interact differently with the entire cementitious system. Some stabilising agents like diutan gum mainly affect the cementitious paste; other stabilising agents like starch tend to interact with the sand fraction and even with the coarse aggregates. Cellulose and guar gum shows more diverse performances.
Typically stabilising admixtures like polysaccharides are used, when sophisticated rheological properties are adjusted. Therefore, polysaccharides are often used in combination with superplasticisers, which are added to reduce the yield stress of concrete. This can cause interactions, particularly when the stabilising Agent shows a strong tendency to adsorb on particle surfaces. Adsorptive stabilising agents may reduce the amount of adsorbed superplasticisers, thus affecting both viscosity and yield stress, while non-adsorptive stabilising agents mainly affect the plastic viscosity independently of the superplasticiser. Due to the strong influence of superplasticisers on the yield stress, influences of the stabilising agent on the yield stress retreat into the background, so that their major effect is an increase of the plastic viscosity.
The paper provides a comprehensive overview of how different polysaccharide superplasticisers affect cementitious flowable systems and points out the challenges of the combined use of polysaccharides and superplasticisers. Based on rheometric experiments and observations of the hydration process, time dependent effects on the workability as well as of the hydration of cement are presented and discussed.
Corrosion fatigue (CF) of duplex stainless steel (DSS) X2CrNiMoN22-5-3 was investigated in in-situ geothermal conditions of the Northern German Basin (NGB). The influence of the load type on CF behavior of the alloy was examined by applying push/pull and rotating bending cyclic load to failure. The hour-glass shaped specimens with both polished and precisely turned surface finish were tested in corrosion chambers allowing for the permanent circulation of Northern German Basin electrolyte heated to 369 K. Additionally, the influence of a protective cathodic potential on the CF life expectancy was investigated by employing a potentiostat. The rotating bending cyclic load led to a higher CF life expectancy, which decreased with increasing duration of the experiment due to a higher deterioration rate of the material. The application of a cathodic potential caused a significant increase of the CF lifespan from 4.7 x 105 (open-circuit potential (OCP)) to 107 cycles (preset threshold cycle number) for the potential range from USHE = – 450 to – 900 mV. Microstructural analysis of the CF damage revealed horizontal grain attack within corrosion pit cavities, multiple fatigue cracks and preferable deterioration of the austenitic phase.
Using the novel optical measurement technique together with the optical flow algorithm, a twodimensional deformation analysis during welding has been conducted. This technique provides for the first time a measurement of the strain field locally in the immediate vicinity of the assumed solidification front. The described procedure of the opticalmeasurement allows to determine the real martial-dependent values of critical strain and strain rate characterising transition to the hot cracking during laser welding processes. The local critical strain that obtained in the assumed solidification showed that the local critical strain decreases as the strain rate increases. Moreover, this phenomenon has also been shown with results from the CTW-test, since the global strain decreases with an increase in the external strain rate.
The vast experience with the automated, ultrasonic system for the inspection of hollow railway axles used by Deutsche Bahn shows that much smaller flaws are detectable than required. This results in a number of false calls. False calls lead to unnecessary demounting and disassembling of wheelsets, which generates unnecessary additional costs. In order to adjust the sensitivity of the inspection system to reduce the number of false calls without compromising safety, the capability of the system to detect cracks needs to be comprehensively established. This capability can be quantified by using probability of detection (POD) curves for the system. The multi-parameter POD model makes it possible to include several factors that influence the crack detection in the analysis. The analysis presented in this paper shows that crack position, orientation, depth extension, and shape as well as the geometry of the axle all have influence on the ultrasonic response amplitude. For future work, calculation of the POD using multi-parameter POD model with these parameters is planned.
Size and shape are crucial parameters which have impact on the potential of nanoparticles to penetrate cell membranes and epithelial barriers. Current research in nanotoxicology additionally focuses on particle coating. To distinguish between core- and coating-related effects in nanoparticle uptake and translocation, two nanoparticles equal in size, coating and charge but different in core material were investigated.
Silver and iron oxide nanoparticles coated with poly(acrylic acid) were chosen and extensively characterized by small-angle x-ray scattering, nanoparticle tracing analysis and transmission electron microscopy (TEM). Uptake and transport were studied in the intestinal Caco-2 model in a Transwell System with subsequent elemental analysis. TEM and ion beam microscopy were conducted for particle visualization.
Although equal in size, charge and coating, the behavior of the two particles in Caco-2 cells was different: while the internalized amount was comparable, only iron oxide nanoparticles additionally passed the epithelium. Our findings suggest that the coating material influenced only the uptake of the nanoparticles whereas the translocation was determined by the core material.
Knowledge about the different roles of the particle coating and core materials in crossing biological barriers will facilitate toxicological risk assessment of nanoparticles and contribute to the optimization of pharmacokinetic properties of nano-scaled pharmaceuticals.
The cocrystal formation of pyrazinamide (PZA) with malonic acid (MA) was studied in situ. The mechanochemical reaction proceeds via conversion of a crystalline intermediate (PZA:MA II) into the thermodynamically more stable form (PZA:MA I) upon further grinding. The information derived from in situ powder X-ray diffraction (PXRD) enabled the isolation of this new metastable polymorph. On the basis of the PXRD data, the crystal structure of the 1:1 cocrystal PZA:MA II was solved. The polymorphs were further characterized and compared by Raman spectroscopy, solid-state NMR spectroscopy, differential thermal analysis/thermogravimetric analysis, and scanning electron microscopy. Our study demonstrates how monitoring mechanochemical reactions by in situ PXRD can direct the discovery and isolation of even short-lived intermediates not yet accessed by conventional methods.
Korrosionsschutz bekennt Farbe - Schnelltest auf Korrosionsgefahr bei nicht rostenden Stählen
(2017)
In Chemieanlagen ist die Passivschicht von Rohrsystemen und Behältern aus nichtrostendem Stahl nicht nur durch den rauen Produktionsalltag gefährdet. Auch im Neuzustand können Schäden entstehen, bspw. durch Schleifvorgänge oder eine unvollständige Entfernung von Anlauffarben nach dem Schweißen. TÜV SÜD Chemie Service beteiligte sich an der Prüfung eines von der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickelten Korrosionsschnelltests. KorroPads liefern in nur 15 Minuten eine valide Aussage zum Zustand der Passivschicht auf den Werkstoffoberflächen.
In order to study the temporally distributed energy deposition in the formation of laser-induced periodic surface structures (LIPSS) on single-crystalline zinc oxide (ZnO), two-colour double-fs-pulse experiments were performed. Parallel or cross-polarised double-pulse sequences at 400 and 800 nm wavelength were generated by a Mach–Zehnder interferometer, exhibiting inter-pulse delays up to a few picoseconds between the sub-ablation 50-fs-pulses. Twenty two-colour double-pulse sequences were collinearly focused by a spherical mirror to the sample surface. The resulting LIPSS periods and areas were analysed by scanning electron microscopy. The delay-dependence of these LIPSS characteristics shows a dissimilar behaviour when compared to the semiconductor silicon, the dielectric fused silica, or the metal titanium. A wavelength-dependent plasmonic mechanism is proposed to explain the delay-dependence of the LIPSS on ZnO when considering multi-photon excitation processes. Our results support the involvement of nonlinear processes for temporally overlapping pulses. These experiments extend previous two-colour studies on the indirect semiconductor silicon towards the direct wide band-gap semiconductor ZnO and further manifest the relevance of the ultrafast energy deposition for LIPSS formation.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon and can be generated on almost any material upon irradiation with linearly polarized radiation. With the availability of ultrashort laser pulses, LIPSS have gained an increasing attraction during the past decade, since these structures can be generated in a simple single-step process, which allows a surface nanostructuring for tailoring optical, mechanical, and chemical surface properties. In this study, the current state in the field of LIPSS is reviewed. Their formation mechanisms are analyzed in ultrafast time-resolved scattering, diffraction, and polarization constrained double-pulse experiments. These experiments allow us to address the question whether the LIPSS are seeded via ultrafast energy deposition mechanisms acting during the absorption of optical radiation or via self-organization after the irradiation process. Relevant control parameters of LIPSS are identified, and technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Up to now, there exists a lack of methods for the additive manufacturing of voluminous ceramic parts with properties comparable to those of conventionally manufactured ones. A high density after sintering is needed to reach the superior properties of ceramic materials. We have developed a new additive manufacturing method, Laser-Induced Slip casting (LIS), to generate ceramic green bodies with high particle packing density and with virtually no restriction in the particle size of the feedstock, especially in terms of small particles. This is achieved by laser-induced local drying of slurries, with the process resembling many features of the well-established stereolithography, but without the excessive use of polymeric material. Thus, unlike the stereolithography process, the resulting green bodies can be processed like traditionally produced ceramic parts. This method allows large and dense additive-manufactured parts to be obtained from conventional water-based ceramic slurries. As an example, we will demonstrate the application of this novel technique with Si3N4.
Licht ist grüner als Strom
(2017)
An improved method of powder 3D printing leading to dense ceramic parts is presented. The application of powder-based binder jetting 3D printing technologies to technical ceramics is generally limited by the low packing density of the powder and by the need to use a flowable powder. With layer-wise slurry deposition, it is, however, possible to deposit powder beds with high particle packing and furthermore using submicron powders. This method was combined with the binder jetting technology to develop a novel process, named LSD-print. By means of LSD-print, a submicron Al2O3 powder could be processed to produce samples with a density comparable with that of standard pressed samples, both in the green state and after sintering.
Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies.
A test campaign was launched to determine the mechanical properties of the High Luminosity-Large HadronCollider (HL-LHC) 11 T Nb3Sn magnet components. The results can be used to accurately represent the mechanical properties in finite elementmodels that predict the stress and strain distribution in these magnets. Particular attention is paid to anisotropic mechanical behavior of the different magnet materials. Static and dynamic test methods have been applied for determining elastic materials’ behavior, and highly accurate Young’s moduli are obtained with the nondestructive dynamic methods resonance and impulse excitation at ambient temperature and during in situ heat cycles.
Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content.
The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.