BAM-Publica - Publikationsserver der Bundesanstalt für Materialforschung und -prüfung
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Zustandserfassung von Spannbetonschwellen mittels akustischer Methoden
Unterseitige oder innenliegende Risse bzw. Gefügeschäden in Spannbetonschwellen können durch Sichtprüfung häufig nicht festgestellt werden. Mit zerstörungsfreien Prüfverfahren werden diese Schäden und deren räumliche Ausdehnung visualisiert und einer quantitativen Analyse unterzogen. Das Ultraschallverfahren kann zusätzlich die Tiefenlage von Rissen innerhalb der Schwellen feststellen. Auch das Impakt-Echo-Verfahren zeigt im Signalbild eine klare Abhängigkeit vom Schwellenzustand. Durch eine neuartige luftgekoppelte Signalanregung, die keinen mechanischen Kontakt zur Oberfläche benötigt, kann dieses Verfahren auf Prüfzügen bei hohen Fahrgeschwindigkeiten eingesetzt werden
Influences of Surface Properties on the Reflection Intensity - Towards in Situ Monitoring During Early Age Hydration of CEM I
Interlayer bonding in 3D concrete printing is influenced by the hydration progress and surface moisture of the previously printed layer. For effective quality control, continuous in situ monitoring of interlayer surface properties is required. This study investigated reflection intensity as a method for in situ measurements during the hydration of CEM I mixtures with varying retarder contents. Additional factors influencing the reflection intensity are also examined. Two laser line scanners with different wavelengths were used to track hydration over 72 h. Vicat tests and isothermal calorimetry served as reference methods. Across all the mixtures, the reflection intensity exhibited a repeatable pattern with five different stages. A sharp increase in intensity during the third stage was consistent with the acceleration period of hydration. These findings suggest that reflection intensity measurements could serve as a promising tool for evaluating interlayer bonding in 3D concrete printing
Influence of the calcination method on the transformations and the reactivity of calcined low-kaolinitic clays
This study investigates the calcination of low-grade kaolinitic clays containing high proportions of 2:1 clay minerals using two different methods: rotary kiln and fluidized bed calcination. The objective was to evaluate their potential as supplementary cementitious materials. The results demonstrate that even clays with low kaolinite content, when processed in a rotary kiln, exhibit pozzolanic properties suitable for cement replacement. Furthermore, fluidized bed calcination proved to be an energy-efficient alternative, achieving considerable dehydroxylation within just 30 min of calcination. This indicates the potential for substantial energy savings compared to conventional calcination techniques. However, further optimization of the process conditions is required to maximize reactivity and industrial applicability. The findings contribute to the ongoing development of sustainable cementitious materials by utilizing widely available, 2:1 clay mineral-dominated resources
Characterization of temperature influence on the structural build-up of 3D printed concrete
3D concrete printing technologies enhance design freedom while reducing material use and costs without the need for formwork. Thereby, structural build-up is the key property governing stability and early strength evolution of 3D printed concrete after placement. Structural build-up is influenced by various factors, i.e., environmental conditions such as temperature. In this paper, the influence of ambient temperature on structural build-up was investigated through experimental and numerical approaches. Three experimental setups (small amplitude oscillatory shear, constant shear rate, and small amplitude oscillatory extensional tests) were applied to materials of increasing complexity under varying temperature conditions. A common modeling framework based on the maturity approach was developed to capture the time and temperature evolution. A stochastic framework was employed to estimate the unknown model parameters using experimental data. Experimental results demonstrate a significant temperature influence on structural build-up, consistent across all test setups and materials. The calibrated models successfully predict the structural build-up under different temperatures, confirming the applicability of the maturity approach to rheological parameters at early age. Furthermore, the stochastic parameter estimation allows a correct quantification of the uncertainties, enhancing model reliability. The comparison of two time evolution formulations indicates that a model with an additional linear stage is required for predicting the increase of the storage moduli (
G
′
,
E
′
). In conclusion, the study demonstrates that temperature significantly affects the structural build-up, and that the proposed modeling approach allows to predict this behavior
Quantitative micro-XRF combined with X-ray imaging reveals correlations between Zn concentration and dentin tubule porosity across entire teeth
Bony materials are biogenic composites of protein fibers and mineral that create hierarchical structures. In the case of teeth, dentin is the main component and similar to other bones, it contains porosity at multiple length scales. It is traversed by micron-sized hollow channels known as dentinal tubules, essential for temperature and pain sensation. Tubule density and thus porosity vary throughout the macroscopic three-dimensional (3D) structure, with porosity increasing toward the pulp. The different densities in teeth are easily revealed non-destructively in 3D by X-ray imaging using computer tomography (CT). Yet elemental composition analysis is more difficult to obtain from within the centimeter-sized heterogeneous bulk material. We describe an approach of merging CT measurements of healthy, intact bovine teeth with micro-X-ray fluorescence (micro-XRF) images of matching serially sectioned slices. Through the combination of multi-resolution quantitative CT measurements with elemental mass fraction derivation, gradients in density and element distributions such as calcium (Ca), phosphorus (P), and zinc (Zn) are revealed across entire teeth in 3D. While the main constituents (Ca and P) are homogeneously distributed in the matrix, Zn concentration increases significantly and exponentially toward the pulp. We find an inverse association between dentin tissue density and Zn concentration localizing this element in or around tubules. Our data serve as a quantitative reference for density and Zn mass fractions in healthy, neither carious nor hypermineralized dentin, as a basis for comparisons across species in health and disease states
Unveiling aging mechanisms of electrolytes in commercial end-of-life lithium-ion batteries
In this study, 77 end-of-life (EOL) commercial lithium-ion batteries (LIBs) of various formats were systematically analyzed to investigate electrolyte degradation and the influence of pristine electrolyte compositions on aging behavior. Comprehensive chemical characterization was conducted using targeted and non-targeted mass spectrometry (MS), employing LC-MS/MS, GC-MS, and high-resolution MS (HRMS). This integrated approach enabled the identification of confirmed pristine components and complex degradation products. The results show that rechargeable pouch and cylindrical cells often deviate from conventional model systems, containing mixed lithium salt anions, ionic liquids (ILs), and high concentrations of triflates, triflimides, and bis(fluorosulfonyl)imide (FSI). These function as solvents, salts, or safety-enhancing additives. Specific IL degradation products were identified, and hypotheses formulated on previously unreported pathways. Furthermore, a novel series of oligomerization products of propylene carbonate (PC) was detected. In contrast, non-rechargeable coin cells revealed widespread use of per- and polyfluoroalkyl substances (PFAS) in their original electrolytes. Based on ex situ analyses, hypothetical PFAS degradation mechanisms are proposed here for the first time. The absence of carbonate oligomers and lithium salt-derived products, alongside the presence of standard carbonates, indicates lithium counterion coordination as a key factor in Lewis acid-catalyzed degradation. This study offers valuable insights into real-world battery aging
Hydrogen-assisted cracking: A deep learning approach for fractographic analysis
Hydrogen handling equipment suffers from interaction with their operating environment, which degrades the mechanical properties and compromises component integrity. Hydrogen-assisted cracking is responsible for several industrial failures with potentially severe consequences. A thorough failure analysis can determine the failure mechanism, locate its origin, and identify possible root causes to avoid similar events in the future. Postmortem fractographic analysis can classify the fracture mode and determine whether the hydrogen-metal interaction contributed to the component’s breakdown. Experts in fracture classification identify characteristic marks and textural features by visual inspection to determine the failure mechanism. Although widely adopted, this process is time-consuming and influenced by subjective judgment and individual expertise. This study aims to automate fractographic analysis through advanced computer vision techniques. Different materials were tested in hydrogen atmospheres and inert environments, and their fracture surfaces were analyzed by scanning electron microscopy to create an extensive image dataset. A pre-trained Convolutional Neural Network was finetuned to accurately classify brittle and ductile fractures. In addition, Grad-CAM interpretability method was adopted to identify the image regions most influential in the model’s prediction and compare the saliency maps with expert annotations. This approach offered a reliable data-driven alternative to conventional fractographic analysis
Breaking down phenylurea herbicides: advanced electrochemical approaches for environmental degradation and remediation
Phenylurea herbicides (PUHs) represent one of the most extensively used herbicide families in agriculture worldwide. While effective for weed control, their environmental persistence, bioaccumulation potential, and formation of toxic metabolites raise significant environmental concerns. This review examines current electrochemical strategies for degrading phenylurea herbicides, with special emphasis on electrochemical oxidation (EC), photoelectrochemical processes (PEC), electro-Fenton (ECF) and photo-electro-Fenton (PECF), with particular attention to the various reactor configurations and their operational mechanisms. A critical innovation of this review lies in its systematic parameter assessment framework, which categorizes nine key operational parameters across all electrochemical degradation methods: electrode material, catalyst type, cell configuration, radiation source, operating conditions (pH, current density, temperature), removal efficiency, mineralization rate, degradation kinetics, identified intermediates, and Energy consumption. For each technique, we highlight which parameters are essential, important, critical, or non� applicable, providing a structured framework to guide future experimental design. Selected case studies are presented to illustrate practical applications and performance outcomes. The review concludes with acritical analysis of current knowledge gaps and future research avenues that could enhance the sustainability, efficiency, and scalability of electrochemical remediation technologies. This work is intended as a comprehensive resource for environmental chemists, analytical scientists, and remediation engineers committed to addressing phenylurea herbicide contamination
Parameter estimation in dynamic multiphase liquid–liquid equilibrium systems
Modeling dynamic systems with a variable number of liquid phases is a challenging task, especially in scenarios where the model is designed for optimization tasks such as parameter estimation. Although there exist methods to model the appearance and disappearance of liquid phases in dynamic systems, they usually require integer variables. In this work, the smoothed continuous approach (SCA) is developed for use with a large number of solvers, since it relies only on continuous variables. To demonstrate the applicability of the new method, the SCA is then applied to model the batch esterification of acetic acid with 1-propanol to water and propyl acetate, and to estimate the reaction parameters. Since the mixture may separate into two liquid phases during the course of the reaction, the parameters are estimated with information on the liquid compositions of both separated liquid phases, which improves the accuracy of the parameter estimates and opens new possibilities for optimal experimental design
Precipitate size evolution in an ultrafine-grained magnesium-manganese alloy
Precipitate size evolution during room temperature high-pressure torsion (HPT) of a Mg-1.35wt.%Mn alloy was studied using scanning transmission electron microscopy (STEM) and Small-/Wide-angle X-ray scattering (SAXS/WAXS). The volume fraction of the nm-scale α-Mn particles increased with applied strain, however small angle X-ray scattering (SAXS) indicated that the majority of manganese remained in solution even after 10 HPT rotations, indicating that the reaction progress is still limited by the diffusivity of Mn. Analysis of the precipitate size distribution determined that the mean particle size did not increase over the course of HPT. This, in combination with the precipitate size distribution suggested that precipitate growth was subject to interfacial rather than diffusional control