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Chemical analysis of commercial functionalized graphene along the production process
No full textGraphene has found widespread commercial use, particularly in flexible electronics and coatings for substrates such as paper and textiles, in the form of suspensions and inks (Zhang et al., 2017). Functionalization of graphene allows fine-tuning of properties like electrical conductivity. Structural and chemical features of graphene materials are typically analyzed by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). While Raman spectroscopy plays a critical role in identifying the presence of graphene and characterizing its structural defects (Pollard et al., 2017), XPS examines the chemistry of graphene. This study investigates three types of graphene materials — graphene (unfunctionalized, G-graphene), fluorine-functionalized graphene (F-graphene), and nitrogen-functionalized graphene (N-graphene) — across three physical forms: powders, suspensions, and embedded in inks. Functionalization was performed via plasma treatment of G-graphene with fluorine or ammonia gases. Suspensions were obtained by dispersing powders in distilled water, while inks were formulated using diacetone alcohol, carbon black, and graphene. Raman spectroscopy analysis confirmed the graphitic nature of all materials and revealed differences in defect density across different forms. The characteristic D, G, and D’ bands varied in relative intensity, offering insight into structural integrity and functionalization effects. XPS measurements examined core-level spectra (C 1s, F 1s, N 1s), revealing chemical bonding environments and hybridization states, including the sp² and sp³ states. A notable decline in fluorine content in F-graphene suspensions and inks, relative to powders, was observed. Existence of organic fluorine and total absence of metallic fluorine were observed. Raman spectroscopy and XPS data provided a correlated view of structural and chemical evolution through the graphene production chain (Figure 1)
Computational modeling of temperature compensation for eddy current testing during PBF-LB/M
No full textThe laser powder bed fusion (PBF-LB/M) process enables the production of highly customized parts with complex geometries. However, the mechanical performance of additively manufactured parts can be compromised by the presence of microstructural inhomogeneities. To address this issue, a reliable process monitoring tool is required to detect these flaws and improve part quality. Eddy current testing presents a promising solution for such monitoring. However, the high temperature gradients within the manufactured specimen affect the electrical conductivity of the material, which, in turn, influences the eddy current testing performance. Therefore, accurately predicting the temperature distribution is essential for reliable flaw detection, which is the focus of this work.
In this study, a Finite Element (FE) transient thermal model is developed to predict the temperature field in multipart build jobs. In this model, scan vectors are grouped into clusters based on their timestamps, enabling the homogenization of thermal loads from multiple scan vectors. When a single cluster is used, the thermal load is applied to the entire layer in a single step. Increasing the number of clusters per layer — and thus the number of steps — enhances the accuracy of temperature predictions. This approach allows for optimizing the trade-off between modeling accuracy and computational efficiency. The study evaluates the prediction accuracy required for eddy current testing and investigates the optimal number of clusters (i.e., the adequate level of homogenization) needed to achieve this accuracy. The model predictions are validated through comparison with thermography images and thermocouple measurements. Finally, the concept of eddy current testing with simulation-based temperature compensation is evaluated on specimens with simple geometries
Laserinduzierte Plasmaspektroskopie (LIBS) im Bauwesen: Anwendungen, Potenziale und aktuelle Entwicklungen
No full textDie laserinduzierte Plasmaspektroskopie (LIBS) hat sich in den letzten Jahrzehnten als leistungsstarke Methode zur Materialcharakterisierung etabliert und bietet insbesondere im Bauwesen vielversprechende Anwendungsmöglichkeiten. Im Vergleich zur klassischen Nasschemie, die oft zeitaufwendig ist und einen hohen Laboraufwand erfordert, zeichnet sich LIBS durch Schnelligkeit, minimale Probenvorbereitung und das Potenzial zur mobilen Anwendung aus.
Im Rahmen des Vortrags wird das im Jahr 2022 vom UA des FA ZfP im Bauwesen veröffentlichte DGZfP-Merkblatt B14 „Quantifizierung von Chlorid in Beton mit der laserinduzierten Plasmaspektroskopie (LIBS)“ vorgestellt und dessen Kerninhalte erläutert. Darüber hinaus werden aktuelle Themen präsentiert, die derzeit im UA von verschiedenen Partnern bearbeitet werden. Dazu gehören unter anderem der Einsatz von LIBS zur Elementanalyse von Schwefel im Zusammenhang mit biogener Schwefelsäurekorrosion sowie wissenschaftliche Fragestellungen wie die Identifizierung von Zementarten und -gehalten im Beton.
Ein weiteres Highlight des Vortrags ist ein aktuelles multidisziplinäres Projekt, das den Einsatz von LIBS in Kombination mit hyperspektraler Bildgebung zur automatisierten Sortierung von Bau- und Abbruchabfällen untersucht.
Ziel des Vortrags ist es, einem breiten Fachpublikum die Potenziale von LIBS im Bauwesen näherzubringen und die Diskussion über zukünftige Anwendungen und Entwicklungen anzuregen
Component test for the assessment of in-service welding on/onto pressurized hydrogen pipelines
No full textHydrogen is seen as the energy carrier of the future. Therefore a reliable infrastructure to transport hydrogen in a large scale is needed. A so called European hydrogen backbone out of long distance transmission pipelines is planned by European countries to create a hydrogen transport infrastructure. Due to economic reasons this will be achieved by new build pipelines such as repurposed natural Gas (NG) pipelines, converted to hydrogen useage. A general suitability for hydrogen service of low alloyed pipeline steel, as it is used for NG service today, is given. But in case of necessary in-service welding procedures in terms of e.g. hot-tapping and stoppling, the risk of a critical hydrogen uptake into the pipe materials due to much higher temeperatures while welding and the possibility of hydrogen embrittlement (HE) needs to be closely investigated. The presentation gives an overview of the current H2-SuD project, investigating the feasability of in-service welding on future hydrogen pipelines. Therefore, component-like demonstrators were developed to test (I) the additional hydrogen uptake due to in-service welding under hydrogen pressure and (II) to measure the temperature field due to different welding parameters and demonstrator geometries, especially on the inner pipe wall surface. Collected data will be used to validate a numerical simulation of the thermal field and additionally the hydrogen diffusion in the pipeline material
Mechanochemical ZIF-9 formation: in situ analysis and photocatalytic enhancement evaluation
No full textEfficient treatment of persistent pollutants in wastewater is crucial for sustainable water management and environmental protection. This study addresses this challenge by investigating the mechanochemical synthesis and photocatalytic performance of ZIF-9, a cobalt-based zeolitic imidazolate framework. Using synchrotron-based powder X-ray diffraction, we provide real-time insights into the formation dynamics of ZIF-9 during mechanosynthesis. Our results show that mechanochemically synthesised ZIF-9 exhibits superior photocatalytic activity compared to its solvothermally prepared counterpart, achieving a 2-fold increase in methylene blue degradation rate. This research not only advances our understanding of the synthesis and properties of ZIF-9, but also demonstrates the potential of mechanochemical approaches in the development of high-performance, sustainably produced materials for water treatment and other environmental applications
Effect of Ti and Nb on hydrogen trapping in welded S690 HSLA steel and effect on delayed cold cracking
No full textFine-grain, high-strength, low-alloy (HSLA) structural steels with yield strengths > 600 MPa are now the state of the art in construction applications such as mobile cranes and civil engineering. HSLA grades derive their strength from a combination of specific heat treatment and the underlying chemical composition. In this context, Ti or Nb are essential to obtain a fine-grained microstructure as well as the necessary carbides or nitrides for precipitation strengthening. In this context, the specific effect of Ti or Nb-rich compounds on hydrogen trapping and diffusion is well known for special laboratory cast alloys, but unknown for realistic steel compositions. For this reason, a series of S690Q-based alloys were synthesized, close to a real steel composition, but with well controlled Ti or Nb additions in different amounts. Specimens were obtained from these alloys by electrochemical discharge machining (EDM). The specimens were tested using the well-established electrochemical permeation technique. From the experimental results, the hydrogen diffusion coefficients and the analytical subsurface hydrogen concentration were calculated. In addition, the hydrogen trapping behavior at elevated temperatures was interpreted by thermal desorption analysis (TDA) using different heating rates of hydrogen charged samples. The results showed that in contrast to metallurgically "pure" laboratory cast alloys, realistic chemical compositions were similar in their hydrogen trapping behavior, despite some small differences. All investigated steel grades exhibited shallow and reversible hydrogen trapping, regardless of their chemical composition. Of course, the experiments only allowed the calculation of effective diffusion coefficients and trapping energies, which represent an average of the entire microstructure. Nevertheless, HSLA steels are typically joined by arc welding, which includes the risk of delayed hydrogen assisted cracking. From the point of view of welding practice, however, a more or less identical hydrogen diffusion behavior means that no special "metallurgically specific", justifiable measures need to be considered, despite the well-established processes such as "soaking" or dehydrogenation heat treatment. Of course, a closer look at the heat-affected zone (HAZ) or the weld metal of the specific welds is necessary. However, especially in the case of thick-walled welds, it is assumed that the weld metal and HAZ are similar to the base material due to the multi-layer welding, which results in multiple annealing cycles of the weld metal and HAZ
Geometric Parameterization and Analysis of Thin-Walled Additively Manufactured Triply Periodic Minimal Surface Structures
No full textAdditive manufacturing (AM) has emerged as a transformative technology for fabricating meta-materials with intricate geometries and tunable macroscopic properties, enabling broad applications across fields such as engineering and biomedicine. A well-known challenge in harnessing the full potential of AM is the tendency of the process to introduce geometric imperfections into printed objects. Such deviations can impact the desired mechanical behavior and performance, which is typically predicted using physicsbased simulations that assume idealized nominal geometries. Therefore, analyzing the “as-is” geometry of AM structures is crucial to ensure the reliability of printed components and their simulators [1, 2]. This work centers on the geometric analysis of thin-walled additively manufactured Triply Periodic Minimal Surface (TPMS) structures. We demonstrate the sensitivity of solid-element-based Finite Element (FE) models to geometric imperfections, highlighting the need to incorporate geometric details of asprinted objects into simulations. To manage the extensive geometric variability and deviations inherent in printed specimens, we propose a regularization approach based on two key geometric descriptors, namely “mid-surface position” and “wall thickness”. These features offer two benefits. First, they provide meaningful metrics for quantitatively comparing printed and nominal geometries. Secondly, they enable the construction of shell-based FE models for thin-walled structures, enriched by the features of the actual printed geometry. One advantage of such shell-based FE models is its significantly lower computational cost compared to a solid FE model, enabling a more efficient incorporation of uncertainty within the estimated geometric features. We demonstrate the procedure for extracting and estimating the two geometric parameters for real printed specimens, leveraging computer tomography (CT) imaging and the derived Signed Distance Field. The advantages of integrating these estimated geometric features into FE simulations are demonstrated through a series of analyses based on real printed specimens
Digital Certificates: Enabling Automation in Quality Assurance and Metrological Traceability
No full textAutomation in the metrological traceability of measurements bears high potential for a more effective quality management with less human interaction and reduced risks from manual data processing. For this purpose all metrological and administrative information in quality certificates must be provided in a fully machine-readable and machine-interpretable form. Following the well-established approach of dig-ital calibration certificates (DCCs) also other digital quality certificates are currently under development
Potentiometric and Optical Titration for Cost- Efficient Quantification of Surface Functional Groups on Silica Nanoparticles
No full textSurface chemistry of engineered nanomaterials (NMs) plays a critical role not only in determining their interactions with the environment but also in their stability, safety, and functionality across diverse applications ranging from catalysis to biomedicine. Accurate quantification of surface functional groups (FGs) is therefore essential for quality control, risk assessment, and performance optimization.[1] However, many existing analytical techniques are either cost-intensive, require specialized instrumentation, or lack scalability for routine use.
In this study, we present a comparative evaluation of potentiometric and optical titration as two simple, cost-efficient, and automatable methods for quantifying surface functional groups on a variety of surface-modified silica nanoparticles (SiO₂ NPs). These NPs were chosen as they are among the most frequently utilized engineered NMs in the life and material sciences.
Potentiometric titration, based on pH monitoring during acid-base neutralization, offers a direct and label-free approach to determine the total amount of FGs. Optical titration provides a complementary method with potential for high-throughput screening. To examine the accuracy and robustness of our stepwise-optimized workflows and the achievable relative standard deviations (RSDs), measurements were performed by multiple operators in two laboratories. Method validation was conducted through cross-comparison with traceable, chemo-selective quantitative nuclear magnetic resonance spectroscopy (qNMR) and thermogravimetric analysis (TGA). A comparison with optical assays highlights the importance of measuring both quantities for comprehensive characterization of surface-modified NMs.[2]
A combined NM surface analysis using optical assays and pH titration will simplify quality control of NM production processes and stability studies, and can yield large datasets for NM grouping in sustainable and safe(r)-by-design studies
Assessment of prestress loss in a large-scale concrete bridge model under outdoor condition
No full textThe presentation shows that subtle variations in coda wave velocity can capture minor temperature effects, offering a good understanding of how a outdoor prestressed concrete structure responds to environmental conditions over time.
Ultimately, this work contributes to development of more comprehensive and resilient structural health monitoring strategies for prestressed concrete infrastructure