Ingenieurwissenschaften und zugeordnete Tätigkeiten
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- Korrosionsschnelltest (6)
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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.
Residual stresses of welds become more and more important influencing cold cracking as well as the fatigue life of welded components. Low transformation temperature (LTT) filler materials offer the opportunity to alter the residual stresses already during the welding process by means of ad- justed martensite phase transformation temperature (MS). In the current paper, welding residual stresses are studied putting the focus on MS while joining heavy steel sections with a thickness of 20 and 25 mm, respectively. The residual stress state was determined at the top surface using X-ray diffraction as well as in the bulk by neutron diffraction. The results com- pare the residual stresses present in a conventional weld and LTT welds when multi-pass welding of large-scale compo- nents was applied. Repeated phase transformation in the case of the LTT weld is more vital for the residual stresses present in the real-life-like joints. This accounts for the top surface in longitudinal direction but is most pronounced for the bulk of the welds. Detrimental tensile residual stresses are mainly re- duced in the bulk in comparison to a conventional filler wire even in multi-pass welds of thick steel sections.
For the damage assessment of reinforced concrete structures the quantified ingress profiles of harmful species like chlorides, sulfates and alkali need to be determined. In order to provide on-site analysis of concrete a fast and reliable method is necessary. Low transition probabilities as well as the high ionization energies for chlorine and sulfur in the near-infrared range makes the detection of Cl I and S I in low concentrations a difficult task. For the on-site analysis a mobile LIBS-system (k = 1064 nm, Epulse ≤ 3 mJ, t = 1.5 ns) with an automated scanner has been developed at BAM. Weak chlorine and sulfur signal intensities do not allow classical univariate analysis for process data derived from the mobile system. In order to improve the analytical performance multivariate analysis like PLS-R will be presented in this work. A comparison to standard univariate analysis will be carried out and results covering important parameters like detection and quantification limits (LOD, LOQ) as well as processing variances will be discussed (Allegrini and Olivieri, 2014 [1]; Ostra et al., 2008 [2]). It will be shown that for the first time a low cost mobile system is capable of providing reproducible chlorine and sulfur analysis on concrete by using a low sensitive system in combination with multivariate evaluation.
Ultrasonic echo testing is widely used in non-destructive testing in civil engineering to investigate concrete structures, to measure thickness, and to locate and characterise built-in components or inhomogeneities. Currently, synthetic aperture focusing techniques are mostly used for imaging. These algorithms are highly developed but have some limitations. For example, it is not possible to image the lower boundary of built-in components like tendon ducts or vertical reflectors. We adopted reverse time migration for non-destructive testing in civil engineering in order to improve the imaging of complicated structures in concrete. By using the entire wavefield, including waves reflected more than once, there are fewer limitations compared to synthetic aperture focusing technique algorithms. As a drawback, the required computation is significantly higher than that for the techniques currently used.
Simulations for polyamide and concrete structures showed the potential for non-destructive testing. The simulations were followed by experiments at a polyamide specimen. Here, having acquired almost noise-free measurement data to test the algorithm, we were able to determine the shape and size of boreholes with sufficient accuracy. After these successful tests, we performed experiments at a reinforced concrete foundation slab. We obtained information from the data by reverse time migration, which was not accessible by traditional imaging. The imaging of the location and structure of the lower boundary of the concrete foundation slab was improved. Furthermore, vertical reflectors inside the slab were imaged clearly, and more flaws were found. It has been shown that reverse time migration is a step forward in ultrasonic testing in civil engineering.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron backscatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
This article reports on the characterization of four superparamagnetic iron oxide nanoparticles stabilized with dimercaptosuccinic acid, which are suitable candidates for reference materials for magnetic properties. Particles p1 and p2 are single-core particles, while p3 and p4 are multi-core particles. Small-angle X-ray scattering analysis reveals a lognormal type of size distribution for the iron oxide cores of the particles. Their mean radii are 6.9 nm (p1), 10.6 nm (p2), 5.5 nm (p3) and 4.1 nm (p4), with narrow relative distribution widths of 0.08, 0.13, 0.08 and 0.12. The cores are arranged as a clustered network in the form of dense mass fractals with a fractal dimension of 2.9 in the multi-core particles p3 and p4, but the cores are well separated from each other by a protecting organic shell. The radii of gyration of the mass fractals are 48 and 44 nm, and each network contains 117 and 186 primary particles, respectively. The radius distributions of the primary particle were confirmed with transmission electron microscopy. All particles contain purely maghemite, as shown by X-ray absorption fine structure spectroscopy
Scattering on scattering
(2017)
Rostfreie Stähle werden in prozesstechnischen Anlagen oft extremen Umgebungsbedingungen ausgesetzt. Eine schützende Passivschicht an der Oberfläche nichtrostender Stähle sorgt dafür, dass es zu keiner Materialauflösung kommt. Wenn diese unvollständig oder beschädigt ist, kann es zu Komplikationen kommen. Lesen Sie im Artikel, wie die von TÜV SÜD Chemie Service erprobte Methode funktioniert, mit der die Passivschicht überprüft werden kann.
At the core of luminescence color and lifetime Tuning of rare earth doped upconverting nanoparticles (UCNPs), is the understanding of the Impact of the particle architecture for commonly used sensitizer (S) and activator (A) Ions. In this respect, a series of core@Shell NaYF4 UCNPs doped with Yb3+ and Ho3+ ions are presented here, where the same dopant concentrations are distributed in different particle architectures following the scheme: YbHo core and YbHo@..., ...@YbHo, Yb@Ho, Ho@Yb, YbHo@Yb, and Yb@YbHo core-Shell NPs. As refealed by quantitative steady-state and time-resolved luminescence studies, the relative spatial Distribution of the A and S ions in the UCNPs and their protection from surface quenching has a critical Impact on ther luminescence characteristics. Although the increased amount of Yb3+ Ions boosts UCNP Performance by amplifying the Absorption, the Yb3+ ions can also efficiently dissipate the energy stored in the material through energy Migration to the surface, thereby reducing the Overall energy Transfer Efficiency to the activator ions. The results provide yet another proof that UC Phosphor chemistry combined with materials Engineering through intentional core@shell structures may help to fine-tune the luminescence Features of UCNPs for their specific future applications in biosensing, bioimaging, photovoltaics, and Display technologies.
Polar semiconductor materials enable a variety of classic and quantum-light sources, which are optimized continuously. However, one key problem—the inherent electric crystal polarization of such materials—remains unsolved and deteriorates the radiative exciton decay rate. We suggest a sequence of reverse interfaces to compensate these polarization effects, while the polar, natural crystal growth direction is maintained. Former research approaches, like growth on less-polar crystal planes or even the stabilization of unnatural phases, never reached industrial maturity. In contrast, our concept provides a way for the development of ultrafast devices based on established growth processes for polar materials, while the electric potential landscape becomes adjustable.
Anlagenkomponenten aus nichtrostendem Stahl sind durch eine Passivschicht auf der Oberfläche vor Korrosion geschützt. Ist diese unvollständig ausgebildet oder beschädigt, geht der Schutz verloren.
Hohe Investitionen für Reparaturen und Instandhaltung können die Folge sein. TÜV Süd Chemie Service beteiligte sich an der Prüfung eines von der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickelten Verfahrens zur Charakterisierung der Korrosionsbeständigkeit der Passivschicht. Der KorroPad-Schnelltest liefert in nur 15 Minuten ein valides Prüfergebnis.
Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry.
First single crystal fibers of cerium doped Strontium yttrate were fabricated using the laser-heated pedestal growth technique. Through thermodynamic Equilibrium calculations and by high-temperature mass spectrometry suitable growth conditions could be determined. The atmosphere played an important role during crystallization. It affected the composition shift, on the one hand, and the valence state of cerium, on the other hand. These dependencies can be explained by combining X-ray diffraction, elemental analysis, and optical spectroscopy. Crystallization in slightly reducing nitrogen atmosphere proved to be a reasonable choice, because evaporation is suppressed and trivalent cerium is stabilized. Strong green emission that depends on the Oxygen fugacity during crystallization could be excited using UV light. Optical properties of SrY2O4:Ce3+ were measured for the first time.
Recent advances in our understanding of CaCO, nucleation from solution have provoked new and challenging questions. We have studied CaC03 formation using precipitation by carbonate ester hydrolysis which ensures precipitation from a strictly homogeneous solution state and allows “titrating” carbonate to a solution with a given Ca2+ concentration on a timescale suited for kinetic studies. Nucleation and crystallization were traced by combining dynamic light Scattering (DLS) and transmission electron microscopy (TEM). DLS served as in situ technique to identify the nucleation time, to monitor particle size evolution, to discriminate different precipitation mechanisms and to validate reproducibility. TEM snapshots taken during different stages of the precipitation process identified different phases and morphologies. At a high level of supersaturation homogeneous nucleation in solution led to the formation of amorphous CaC03 particles (diameter=30 nm), which transformed via vaterite to calcite. Nucleation occurred uniformly in solution which appears to be unique for the CaC03 System. In the presence of Na-polymethacrylate (Na-PMA), heterogeneous nucleation was suppressed and Ca-polymer aggregates were formed in the prenucleation stage. Beyond a critical threshold supersaturation CaC03 particles formed in solution outside of these aggregates. The nucleation process resembled that without additive, indicating that Na-PMA exerts only a minor effect on the CaC03 nucleation. In the postnucleation stage, the polymer led to the formation of extended liquid-like networks, which served as a precursor phase for solid ACC particles that formed alongside the network.
Complex formation and the coordination of zirconium with acetic acid were investigated with Zr K-edge extended X-ray absorption fine structure spectroscopy (EXAFS) and single-crystal diffraction. Zr K-edge EXAFS spectra show that a stepwise increase of acetic acid in aqueous solution with 0.1 M Zr(IV) leads to a structural rearrangement from initial tetranuclear hydrolysis species [Zr4(OH)8(OH2)16]8+ to a hexanuclear acetate species Zr6(O)4(OH)4(CH3COO)12. The solution species Zr6(O)4(OH)4(CH3COO)12 was preserved in crystals by slow evaporation of the aqueous solution. Single-crystal diffraction reveals an uncharged hexanuclear cluster in solid Zr6(μ3-O)4(μ3-OH)4(CH3COO)12·8.5H2O. EXAFS measurements show that the structures of the hexanuclear zirconium acetate cluster in solution and the solid state are identical.
Currently great effort is made to find materials and technologies for the recycling of phosphate from wastewater.
Herein, we present an in-depth study of the Phosphate adsorption mechanism of a promising adsorber material, a Zn−Fe−Zr oxyhydroxide-based nanostructured precipitate. The behavior of the multicomponent nanomaterial, consisting of both crystalline and amorphous parts, is investigated via X-ray absorption fine structure spectroscopy and Mössbauer spectroscopy, revealing the importance of the nanostructured composition for the phosphate adsorption. We found evidence that adsorption takes place especially in the vicinity of iron sites in the amorphous part of the material.
Periodic self-organization of matter beyond the diffraction limit is a puzzling phenomenon, typical both for surface and bulk ultrashort laser processing. Here we compare the mechanisms of periodic nanostructure formation on the surface and in the bulk of fused silica. We show that volume nanogratings and surface nanoripples having subwavelength periodicity and oriented perpendicular to the laser polarization share the same electromagnetic origin. The nanostructure orientation is defined by the near-field local enhancement in the vicinity of the inhomogeneous scattering centers. The periodicity is attributed to the coherent superposition of the waves scattered at inhomogeneities. Numerical calculations also support the multipulse accumulation nature of nanogratings formation on the surface and inside fused silica. Laser surface processing by multiple laser pulses promotes the transition from the high spatial frequency perpendicularly oriented nanoripples to the low spatial frequency ripples, parallel or perpendicular to the laser polarization. The latter structures also share the electromagnetic origin, but are related to the incident field interference with the scattered far-field of rough non-metallic or transiently metallic surfaces. The characteristic ripple appearances are predicted by combined electromagnetic and thermo-mechanical approaches and supported by SEM images of the final surface morphology and by time-resolved pump-probe diffraction measurements.
Photoluminescence techniques are amongst the most widely used Tools in the life sciences, with new and exciting applications in medical diagnostics and molecular Imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for Multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from Instrument-dependent effects, which are also time-dependent due to aging of Instrument-components, and difficulties to measure absolute flourescence entensities. Moreover, scattering Systems require Special measurement geometries and the interest in new optical Reporters with Emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material Performance and the rational designg of new flourophores with improved properties.
Here, we present strategies to versatile method-adaptable liquid and solid flourescence Standards for different flourescence paramters including traceable Instrument calibration procedures and the design of integrating spere setups for the absolute measurements of emission spectra and Quantum yields in the wavelength Region of 350 to 1600 nm. Examples are multi-Emitter glasses, spectral flourescence Standards, and quantum yield Standards for the UV/vis/NIR.
The process of laser cladding has become more important during recent years because of its broad application for cladding, repair or additive manufacturing. In the field of mechanical engineering, one use is the repair of turbine blades. For high quality and reliability of the repaired components, it is necessary to adjust the weld bead geometry to the specific repair task. The bead geometry influences the metallurgical bonding and the degree of dilution as well as the formation of defects like pores or cracks. Therefore, it is important to know the effects of the different parameters on the welding bead. A valuable tool to meet this industrial challenge is the design of experiments (DoE). In this context, the user can choose between a huge number of test plans. Greater Profit of information is expected by a larger test range. In order to confirm the acceptance, a five-step full factorial test plan is compared to a central composite design in this paper. Moreover, the limits of the experimental range are indicated and restrictions can be derived. As the results show, the essential effects are detected with a full factorial test plan as well as with a central composite design. Merely the effect strength could not always be specified unambiguously. On this account and in consideration of cost efficiency, the use of central compound design is recommended in industrial applications.
Stress-induced damage evolution in cast AlSi12CuMgNi alloy with one- and two ceramic reinforcements
(2017)
Two composites, consisting of an as-cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 short fibres and with 7%vol. Al2O3 short fibres + 15%vol. SiC particles were studied. Synchrotron computed tomography disclosed distribution, orientation, and volume fraction of the different phases. In-situ compression tests during neutron diffraction in direction parallel to the fibres plane revealed the load partition between phases. Internal damage (fragmentation) of the Si phase and Al2O3 fibres was directly observed in CT reconstructions. Significant debonding between Al-matrix and SiC particles was also found. Finally, based on the Maxwell scheme, a micro-mechanical model was utilized for the new composite with two ceramic reinforcements; it rationalizes the experimental data, and predicts the evolution of all internal stress components in each phase.