Ingenieurwissenschaften und zugeordnete Tätigkeiten
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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.
Kikuchi diffraction patterns can provide fundamental information about the lattice metric of a crystalline phase. In order to improve the possible precision and accuracy of lattice parameter determination from the features observed in Kikuchi patterns, some useful fundamental relationships of geometric crystal-lography are reviewed, which hold true independently of the actual crystal symmetry. The Kikuchi band positions and intersections and the Kikuchi band widths are highly interrelated, which is illustrated by the fact that all lattice plane trace positions of the crystal are predetermined by the definition of only four traces. If, additionally, the projection centre of the gnomonic projection is known, the lattice parameter ratios and the angles between the basis vectors are fixed. A further definition of one specific Kikuchi band width is sufficient to set the absolute sizes of all lattice parameters and to predict the widths of all Kikuchi bands. The mathematical properties of the gnomonic projection turn out to be central to an improved interpretation of Kikuchi pattern data, emphasizing the importance of the exact knowledge of the projection centre.
Semicrystalline polymers have to be described by a three phase model consisting of a mobile amorphous (MAF), a crystalline (CF), and a rigid amorphous fraction (RAF). For nanocomposites based on a semicrystalline polymer the RAF is due to both the crystallites (RAFcrystal) and the filler (RAFfiller). Polymer nanocomposite based on poly(L-lactide) and MgAl layered double hydroxide nanofiller were prepared.
Due to the low crystallization rate of PLA ist crystallization can be suppressed by a high enough cooling rate, and the RAF is due only to the nanofiller. The MAF, CF, and RAF were estimated by Temperature Modulated DSC. For the first time CF, MAF, RAFcrystal, and RAFfiller could be estimated. It was found, that RAFfiller increases linearly with the concentration of the nanofiller for this system. Furthermore, RAFcrystal is only slightly influenced by the presence of the nanofiller.
Present trends to lightweight design lead to an expanding relevance of high-strength fine-grained structural steels especially in mobile crane constructions. With growing material strength, the challenge for welding fabrication increases, since high loading capacities and safety requirements have to be accomplished. The utilisation of the high strength potential often requires complex constructions associated with high restraint conditions while welding. Increased residual stresses may occur due to superimposing reaction and restraint stresses, which have to be quantified and evaluated to ensure the safety and integrity of high-strength steel constructions. Particularly, the scope of residual stresses has to be taken into account for different effects in the HAZ, notches, weld and base metal. Commonly, conservative assumptions of residual stresses lead to distinct underestimations of the load bearing capacity particularly for welded high-strength steel constructions. This study concludes results of recent works of the researchers regarding the complex interaction among heat control, material and restraint intensity on the residual stress state in welded components. These analyses are extended by further experiments. Based on the obtained major effects, an approach for a welding residual stress assessment regarding component design according to prevailing standards for crane construction, an important application for high-strength steels, is presented.
Effect of different sulphur-based crosslink networks on the nitrile rubber resistance to biodiesel
(2017)
Biodiesel possesses some comparable physical properties to petroleum diesel in addition to its improved environmental benefits. Nonetheless, both fuels differ greatly with respect to their chemical compositions.
Therefore, the compatibility of the materials, which are commonly employed in contact with diesel, must also be assured for biodiesel. This paper assessed the influence of sulphur-based curing systems on the resistance of nitrile rubber to soybean biodiesel. Formulations were prepared using highacrylonitrile-content nitrile rubber by employing a two-level experimental design. The amounts of two different accelerators and sulphur were varied to achieve different types of vulcanisation systems.
Thermal analyses, mechanical tests and microscopy analyses were conducted to evaluate the behaviour of the material after contact with biodiesel. The results showed that the choice of the accelerator played an important role on the resistance of the rubber to the biofuel, and crosslink density was not a key factor with respect to the resistance.
Active antibacterial and antifouling surface coating via a facile one-step enzymatic cross-linking
(2017)
Prevention of microbial contamination of surfaces is one of the biggest challenges for biomedical applications. Establishing a stable, easily produced, highly antibacterial surface coating offers an efficient solution but remains a technical difficulty. Here, we report on a new approach to create an in situ hydrogel film-coating on glass surfaces made by enzymatic cross-linking under physiological conditions. The cross-linking is catalyzed by horseradish peroxidase (HRP)/glucose oxidase (GOD)-coupled cascade reactions in the presence of glucose and results in 3D dendritic polyglycerol (dPG) scaffolds bound to the surface of glass.
These scaffolds continuously release H2O2 as long as glucose is present in the system. The resultant polymeric coating is highly stable, bacterial-repellent, and functions under physiological conditions. Challenged with high loads of bacteria (OD540 = 1.0), this novel hydrogel and glucose-amended coating reduced the cell viability of Pseudomonas putida (Gram-negative) by 100% and Staphylococcus aureus (Gram-positive) by ≥40%, respectively. Moreover, glucose-stimulated production of H2O2 by the coating system was sufficient to kill both test bacteria (at low titers) with >99.99% Efficiency within 24 h. In the presence of glucose, this platform produces a coating with high effectiveness against bacterial adhesion and survival that can be envisioned for the applications in the glucose-associated medical/oral devices.
Mn0.75Ga0.25As crystallites, partially embedded on and fully embedded within a single crystalline matrix of GaAs formed during metal organic vapor phase epitaxy (MOVPE) of Mn-rich (Mn,Ga)As on (001) oriented GaAs wafers. Phase and orientation analysis of these crystallites were performed with scanning nano beam electron diffraction (SNBED). The investigation of plan-view specimens using a liquid nitrogen cooling stage enabled the phase and orientation analysis of partially embedded ferromagnetic a-phase particles. In all specimens the following two orientation relationships (O) between the a-phase particles and the GaAs matrix were determined:
O1:
[1-2.0] Mn0.75Ga0.25As || [110] GaAs and
[10.2] Mn0.75Ga0.25As || [-110] GaAs
O2:
[10.2] Mn0.75Ga0.25As || [110] GaAs and
[1-2.0] Mn0.75Ga0.25As || [-110] GaAs.
The study of cross-sectional specimens enabled the analysis of fully embedded crystallites. It could be unambiguously detected that a fully embedded crystallite has the structure of the atomically ordered monoclinic β' phase. The β' phase crystallite consists of two domains which are related in twin positions to each other. The orientation relations of the different particles are illustrated by color coded stereographic projections.
The main aim of the research was the development of a first valid database for material parameters of earth block masonry (EBM) with particular regard to statistical characteristics. A solid database is needed for the determination of the materials partial safety factor. Therefore, compressive strength tests were carried out with two types of earth blocks and two types of prefabricated earth mortar.
The evaluation has shown that the mean variation of the compressive strength was remarkably less than expected, which indicates high quality standards of the components earth block and mortar with regard to industrial production. Using the reliability method, a partial safety factor for EBM subjected to compression was determined on the basis of these test results. The findings have shown that a common calculation method for EBM based on partial safety factors following the valid masonry construction standard is feasible.
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.
Seitens der Industrie besteht großes Interesse, Polyethylenterephthalat (PET) als Werkstoff für Verpackungen zum Transport von Gefahrgütern einzusetzen, da aufgrund der hohen Fes-tigkeit und Steifigkeit von PET die Wanddicken und somit die Kosten der Verpackungen reduziert werden können. Die Prüfung der Spannungsrissbeständigkeit von Polyethylenformstoffen als Werkstoffe von Verpackungen erfolgt mit Labormethoden unter Verwendung einer Standardflüssigkeit als Prüfmedium für die Spannungsrisse auslösende Wirkung auf Polyethylen (PE), wodurch Zeit und Kosten der Prüfungen reduziert werden.
Ziel dieser Arbeit war es, eine Laborprüfmethode zum Vergleich der Spannungsrissbeständigkeit von PE und PET auf ihre Anwendbarkeit zu prüfen, wie z.B. den Full Notch Creep Test (FNCT). Es wurde untersucht, ob die Prüfkörper aus PE und PET mit umlaufender Kerbe in dieser durch die chemische Industrie entwickelten und von der BAM konzipierten Apparatur auf der Basis des FNCT zu messbaren Ergebnissen unter Einfluss eines Ölsäureamidethoxylates als Netzmittel bei 50 °C führen.
Die Testergebnisse bestätigten die Eignung des Prüfverfahrens für die acht eingesetzten Formstoffe aus PE. Dieses Prüfverfahren konnte nicht für PET angewandt werden, da die Prüfkörper aufgrund der hohen Festigkeit und Steifigkeit des PET beim Kerbvorgang zerbrachen. Die gleiche Aussage konnte für den Nachweis der der Spannungsrissbeständigkeit von Verpackungen, der in der BAM Gefahrgutregel BAM-GGR 015 beschrieben wird, getroffen werden. Die einzige Möglichkeit zum Nachweis der Spannungsrissbeständigkeit von PET besteht in der Durchführung von Stapeldruckprüfungen.
Welding is the most important joining technique and offers the advantage of customizable plate thicknesses. On the other hand, welding causes residual stresses and deformations influencing the load carrying capacity. Their consideration in the design requires simple and fast models. Though welding simulation has contributed to accurately access to these values nowadays, their application to large components remains still in a less practicable range. Nevertheless, many studies emphasized the need to make corrections in recently available simplified models. Especially the influence of residual stresses seems somewhat overestimated in many cases if comparing conventional structural steel S355 and high-strength steel S690. In the age of computer-aided design, an improved procedure to implement weld-inducted imperfections appears overdue. This will be presented in two parts. The first part illustrates the potential influence of post-welding imperfections exemplified for weak axis buckling in comparison with the general method in accordance with Eurocode 3. Residual stresses and initial crookedness were varied systematically in order to produce a scatter band of capacities. An approach to characterize the borders of these imperfections was untertaken before that. The excessive scattering of reduction factors for the load bearing capacity demonstrates the importance of these variables. Results were finally evaluated against advanced simulation models which will be further detailed in part two of this contribution.
Estimation of heat flux parameters during static gas tungsten arc welding spot under argon shielding
(2017)
A multi-physics modelling of a static Gas Tungsten Arc Welding (GTAW) operation has been established in order to estimate the heat flux exchanged between the arc plasma and the work-piece. The heat flux was described with a Gaussian function where two parameters required to be estimated: process efficiency and radial distribution. An inverse heat transfer problem (ihtp) has been developed in the aim to estimate these parameters from experimental data. Levenberg-Marquardt algorithm was used as the regularization method in addition to an iterative process. The experiment consisted in a static spot weld with GTAW process. The weld spot was on for 5 s under Argon shielding gas, 2.4 mm pure tungsten electrode on a SS304L disc. Temperatures were measured with thermocouples and weld pool growth monitored with a high speed camera. The experimental data were used to solve the ihtp what led to values such as 0.7 for process efficiency and average radial distribution of 1.8 mm.
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.
Neutron Bragg-edge imaging was applied for the visualization of a γ-Austenite to α'-martensite phase transformation. In the present study, a super martensitic
stainless steel sample was heated until complete austenitization and was subsequently cooled down to room temperature. The martensitic phase Transformation started at Ms = 190 °C. Using a monochromatic neutron beam with λ = 0.390 nm, the transmitted intensity was significantly reduced during cooling below Ms, since the emerging martensitic phase has a higher attenuation coefficient than the austenitic phase at this wavelength. The phase Transformation process was visualized by filming the transmission images from a scintillator screen with a CCD camera with a temporal resolution of 30 s and a spatial
resolution of 100 µm.
The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction(ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth.
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.
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.
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.
Micrometric surface topologies are required for a wide range of technical applications. While lowered surface features have been used for many years to improve the tribological behavior of contacting surfaces, there are also other fields of application, where the potential of elevated surface features is known, e. g. for metal forming tools. However, the demand for a high wear resistance of these structures often inhibits an industrial application. A solution is offered by structuring techniques that use additional material. A promising approach is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This paper describes the potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces by means of microstructural and topological investigations. Afterwards, results of a wear test are given and different applications for this structuring technique are discussed. It can be shown that dome-shaped or ring-shaped structures on a micrometric scale can be produced with high hardness and wear resistance.
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.