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Bulk metallic glasses (BMG) are amorphous metal alloys known for their unique physical and mechanical properties. In the present study, the formation of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on the Zr-based BMGs Zr46Cu46Al8, Zr61Cu25Al12Ti2, Zr52.5Cu17.9Al10Ni14.6Ti5 (Vit105) and Zr57Cu15.4Al10Ni12.6Nb5 (Vit106) was investigated as a function of their different chemical composition. For this purpose, LIPSS were generated on the sample surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz). The surface topography was characterized by scanning electron microscopy and atomic force microscopy. Moreover, the impact of LIPSS formation on the structure and chemical surface composition was analyzed before and after fs-laser irradiation by X-ray diffraction and X-ray photoelectron spectroscopy as well as by transmission electron microscopy in combination with energy dispersive X-ray spectroscopy. Despite the different chemical composition of the investigated BMGs, the fs-laser irradiation resulted in almost similar properties of the generated LIPSS patterns. In the case of Zr61Cu25Al12Ti2, Vit105 and Vit106, the surface analysis revealed the preservation of the amorphous state of the materials during fs-laser irradiation. The study demonstrated the presence of a native oxide layer on all pristine BMGs. In addition, fs-laser irradiation results in the formation of laser-induced oxide layers of larger thickness consisting of an amorphous ZrAlCu-oxide. The precise laser-structuring of BMG surfaces on the nanoscale provides a versatile alternative to thermoplastic forming of BMG surfaces and is of particular interest for the engineering of functional material surfaces.
Laser-induced breakdown spectroscopy (LIBS) is a spectroscopic method for the analysis of the chemical composition of sample materials. Generally, the measurement of all elements of the periodic table is possible. In particular, light elements such as H, Li, Be, S, C, O, N and halogens can be measured. Calibration with matrix-matching standards allows the quantification of element concentrations. In combination with scanner systems, the two-dimensional element distribution can be determined. Even rough surfaces can be measured by online adjustment of the laser focus. LIBS can also be used on-site with mobile systems. Hand-held systems are available for point measurements.
Common applications include the investigation of material deterioration due to the ingress of harmful ions and their interaction in porous building materials. Due to the high spatial resolution of LIBS and the consideration of the heterogeneity of concrete, the determination of precise input parameters for simulation and modelling of the remaining lifetime of a structure is possible. In addition to the identification of materials, it is also possible to assess the composition for example of hardened concrete, which involves the cement or aggregate type used. Other important fields of application are the detection of environmentally hazardous elements or the material classification for sorting heterogeneous material waste streams during dismantling. Non-contact NDT for “difficult to assess” structures as an example application through safety glass or in combination with robotics and automation are also possible.
In this work, an overview of LIBS investigations on concrete is given based on exemplary laboratory and on-site applications.
The release of hazardous compounds from construction products can harm human health and the environment. To improve the sustainability of construction materials, the leaching of substances from construction products and their potential environmental impact should be assessed. Twenty-seven construction products from different product groups were examined with a combination of standardized leaching tests (dynamic surface leaching test and percolation test) and biotests (algae, daphnia, fish egg, luminescent bacteria, umu and Ames fluctuation tests). To identify the released substances, extensive qualitative and quantitative chemical analyses were performed, including gas chromatographic and liquid chromatographic screening techniques.
Results: Many of the tested eluates caused signifcant ecotoxic efects. Particularly high ecotoxicities were observed for grouts (lowest ineffective dilution (LID) up to 16384) and cork granules (LID up to 24578). The results of ecotoxicity tests allow the prioritization of the eluates that should be subjected to detailed chemical analyses. Organic screening by different methods and ranking the identifed substances based on recorded hazard classification is a suitable approach to identify the relevant toxic substances.
Conclusions: Determining the ecotoxicity of eluates from construction products records the summary effect of all leachable substances. This instrument is especially useful for construction products of complex and largely unknown composition. The ecotoxicological and the chemical–analytical approach complement each other in an ideal way to characterize the potential hazard of eluates from construction products and to identify the environmentally hazardous components in these eluates. Our results confirm that the proposed harmonized methods for testing eluate toxicity are an adequate and applicable procedure to move toward a more sustainable way of building and to reduce toxic effects of construction products in their use phase in the environment.
Due to its large strength-to-weight ratio and excellent biocompatibility, titanium materials are of paramount importance for medical applications, e.g. as implant material for protheses. In this work, the evolution of various types of laser-induced micro- and nanostructures emerging on titanium or titanium alloys upon irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment is studied for various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz). The morphologies of the processed surfaces were systematically characterized by optical and scanning electron microscopy (OM, SEM). Complementary white-light interference microscopy (WLIM) revealed the corresponding surface topographies. Chemical and structural changes were analysed through depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray diffraction (XRD) analyses. The results point towards a remarkable influence of the laser processing parameters on the surface topography, while simultaneously altering the near-surface chemistry via laser-induced oxidation effects. Consequences for medical applications are outlined.
Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels.
Laser-induced breakdown spectroscopy (LIBS) is a combination of laser ablation and optical emission spectroscopy. Due to the possibility of direct measurements on the sample surface with a minimum of sample preparation investigations of building materials can be conducted quite fast. In combination with a scanning technique (translation stage or scanning mirrors head) 2D element distributions of harmful species like chlorides and alkalis are evaluated with a sub-mm resolution. By scanning a surface of typically 100 mm x 100 mm the heterogeneity of the material may be considered. LIBS is capable to identify hot spots in element concentration with a resolution of 0.1 mm or even smaller. A LIBS-system for the on-site application on building materials is, in cooperation with system developers and companies which will use this technique for investigation on real structures, under test at BAM. We present an example. Further work will focus on providing guidelines to establish LIBS as a standard procedure for chemical investigations of building materials.
LIBS is on the step from a laboratory application to on-site analysis. A validated mobile LIBS-system for on-site application on building materials is under development at BAM in cooperation with industrial partners (system developers and companies), who will use this technique for investigation on building structures like bridges and parking decks. The system is designed to measure the content of harmful species like chlorine, sulfur or alkalis, to give the engineer a tool for the estimation of the condition of concrete structures and for quality assurance during concrete repair work on-site. In these work results of on-site measurements on a chloride contaminated bridge are shown. Further work will focus on providing guidelines to establish LIBS as a standard procedure for chemical investigations of building materials.
The laser induced breakdown spectroscopy (LIBS) is a combination of laser ablation and optical emission spectroscopy. Due to the possibility of direct measurements on the sample surface and a minimum of required sample preparation investigations of building materials can be conducted quite fast. In combination with a scanning technique (translation stage or scanning mirrors head) the element distributions are evaluated taking in to account the heterogeneity of the material. This is a significant advantage compared to standard procedures. LIBS measurements are also time and cost saving in comparison to standard methods. The automated measurement procedures minimise the liability for errors. All elements are detectable and after calibration results can be quantified. At BAM LIBS has been successfully applied for the investigation of distribution and transport of different ions in building materials. Quantitative measurements are performed for chlorine, sodium, potassium, sulphur, lithium and hydrogen. Beside this the identification of substances and the evaluation of quantitative ratios by means of an integrated marker are possible. An overview about the principle and the possibilities of LIBS investigations of building materials is presented and typical applications are shown. The LIBS technique is on the step from laboratory application to on-site analyses.