BAM-Publica - Publikationsserver der Bundesanstalt für Materialforschung und -prüfung
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63. DAfStb-Forschungskolloquium in der BAM - Themenblock 1: Chemie der Bindemittel
Aus Gründen des Klimaschutzes werden in den kommenden Jahren mehr Zemente mit verringertem Klinkerfaktor und alternative Bindemittel (klimafreundliche Bindemittel) zum Einsatz kommen. Für ihre sichere und zuverlässige Verwendung ist ein umfangreiches Verständnis der Einflüsse auf die Dauerhaftigkeit der aus ihnen hergestellten Betone notwendig. In jüngerer Zeit sind hierzu insbesondere von Technischen Komitees in RILEM und in der EFC neue Erkenntnisse gewonnen worden, die im Rahmen des 63. DAfStb-Forschungskolloquiums an der BAM (Tagungsband: DOI 10.26272/opus4-61338) im Zusammenhang mit den Beiträgen der BAM zu diesen Ergebnissen
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Exploring INFOTherm and current research
This presentation introduces the INFOTherm project aiming to standardize and improve fiber-optic temperature sensing. Current research focuses on how humidity affects the temperature sensitivity of polyimide-coated fibers
Harmonized tribological testing of polymers in hydrogen
To investigate typical polymer compounds and a potential alternative to be used in hydrogen compressors, tribological tests have been performed with several tribometers in hydrogen atmosphere. The compounds used were a commercially available PEEK matrix with 10 wt-% PTFE, graphite, and short carbon fibers each (supplied by company Polytron), a PPS matrix with 10 wt-% PTFE and graphite (supplied by company MOCOM) and an experimental PA12 matrix with PTFE, chemically coupled with an oleyl alcohol, as additive (supplied by the polymer research institute IPF). For all compounds a steel counter disc (type 316L / 1.4404) with a lapped surface was used in a cylinder on disc setup.
The focus of this work is to study the tribological performance of the polymers in hydrogen atmosphere. Additionally, tests were carried out with up to three different tribometers at two institutions. The challenge to compare and harmonize equipment, procedures, and methods is an important part of the study. This naturally includes the determination of the wear volumes of the polymeric cylinders. Furthermore, selected results of the wear and the resulting change in the contact geometry were compared by FEM simulations and an analytical model
Spannstahlbrücken der Vergangenheit in der Zukunft richtig bewerten
Spannstahlbrücken die in der Vergangenheit mir vergüteten Spannstählen errichtet worden sind können unter ungünstigen Gegebenheiten bei deren Erstellung signifikante Probleme hinsichtlich der Tragfähigkeit bekommen. Im Speziellen kann die wasserstoffinduzierte Spannungsrisskorrosion hier bei der Errichtung der Brückenbauwerke Anrisse an den Spanndrähten erzeugt haben die Jahre später zum Versagen der Brücke führen können. Die Präsentation im Speziellen behandelt den Teileinsturz der Carolabrücke in Dresden
Quantification of hydrogen uptake during in-service hydrogen pipeline welding
Hydrogen must be transported on a large scale from producers to consumers to ensure the energy transition. The necessary pipeline grid is achieved by conversion of the natural gas (NG) grid and building new pipelines. Welding during service as part e.g. of “hot-tapping” is unavoidable for maintenance/repair/expansion. Based on existing studies, the basic material compatibility of (low-alloyed) pipeline steels with hydrogen is postulated. However, this cannot be assumed for the case of in-service welding on pipelines in pressurized condition. The reason is the increased temperature e.g. by preheating and (in particular) during welding of the single passes. As a result, the inner pipeline surface undergoes multiple short-term heating but to high temperatures. In particular, the first passes can result in a temperature close to the austenitic transformation of the material for small wall thicknesses. Both increase the hydrogen uptake into the welded joint. If hydrogen embrittlement is likely to occur, depends on the hydrogen uptake, which must be quantified. For this purpose, welding experiments on pressurized demonstrators were conducted. The hydrogen uptake at 100 bar was compared to reference experiments with nitrogen. A new sample extraction routine for the quantification of the weld-zone specific hydrogen uptake was established. Comprehensive experiments with different steels (P235, L360, L485), wall thicknesses (4.1 mm to 7.8 mm) and diameters (DN50 and DN200) were conducted. In addition, the influence of the welding layer sequence on the hydrogen uptake between single- and multi-layer welds was investigated. Analytical approaches were used to approximate the hydrogen uptake in the respective weld zones. The main findings were that the layer sequence and especially the wall thickness have a large influence on the hydrogen uptake
Measurement of the Lateral Size of Graphene Oxide Flakes by SEM
The progress of the VAMAS interlaboratory comparison Project P13 "Lateral size of graphene oxide flakes by SEM" within the Technical Working Area 41 "Graphene and Related 2D Materials" is presented. The challenges at sample preparation on substrates for accurate measurement and image analysis as well as two different analysis approaches, containing exact guidance how to measure the main descriptors for the lateral size measurement of the imaged graphene oxide flakes with Scanning Electron Microscopy are highlighted. The size and shape distributions as measured by 17 laboratories are showed expressed in size and shape descriptors extracted from SEM images by using two proposed measurement approaches.
The implementation of the results into the corresponding ISO technical specification AWI/TS 23879 is discussed and planned, in relation with the AFM part
Natural language processing for automated workflow and knowledge graph generation in self-driving labs
Natural language processing with the help of large language models such as ChatGPT has become ubiquitous in many software applications and allows users to interact even with complex hardware or software in an intuitive way. The recent concepts of Self-Driving Labs and Material Acceleration Platforms stand to benefit greatly from making them more accessible to a broader scientific community through enhanced user-friendliness or even completely automated ways of generating experimental workflows that can be run on the complex hardware of the platform from user input or previously published procedures. Here, two new datasets with over 1.5 million experimental procedures and their (semi)automatic annotations as action graphs, i.e., structured output, were created and used for training two different transformer-based large language models. These models strike a balance between performance, generality, and fitness for purpose and can be hosted and run on standard consumer-grade hardware. Furthermore, the generation of node graphs from these action graphs as a user-friendly and intuitive way of visualizing and modifying synthesis workflows that can be run on the hardware of a Self-Driving Lab or Material Acceleration Platform is explored. Lastly, it is discussed how knowledge graphs – following an ontology imposed by the underlying node setup and software architecture – can be generated from the node graphs. All resources, including the datasets, the fully trained large language models, the node editor, and scripts for querying and visualizing the knowledge graphs are made publicly available
Hydrogen safety- Dealing with Closed Spaces
This work focuses on the detection and monitoring of hydrogen concentration in closed spaces, to improve safety by developing a sensor network-based leak detection system. This will help in prevention of accumulation of hazardous mixtures. Furthermore, the study details the implementation of a hydrogen sensor network within a container, analysing sensor placement, data collection, and safety improvements
Screening Procedures for Self-Reactive Substances, Differential Scanning Calorimetry-Onset and Heat-Flux Criteria (paper)
We present a new screening procedure for the determination of the thermal stability of potential candidates for the class of self-reactive substances. For the classification of self-reactive substances, elaborate testing is necessary to determine the applicable type, according to the regulations. Annex 6 of the UN Manual of Tests and Criteria permits that the classification procedure for self-reactive substances may be omitted, if the estimated self accelerating decomposition temperature (SADT) is greater than 75 °C for a 50 kg package using an appropriate calorimetric technique, but no technique is described. Based on stationary theories of thermal explosion, we developed a screening approach using differential scanning calorimetry (DSC) onset and heat-flux criteria, respectively, at relevant temperatures. The proposed approach is validated with experimental data
Separation of Indium Phosphide/Zinc Sulfide Core−Shell Quantum Dots from Shelling Byproducts through Multistep Agglomeration
Semiconductor quantum dots (QDs) possess unique electronic and optical properties, making them promising candidates for applications in lightemitting diodes, solar cells, bioimaging, and photocatalysis. Precise control over their size, shape, and chemical and electronic structure is crucial to ensure the desired functional properties and optimize device performance. However, challenges in QD synthesis and post-synthesis modification persist, especially in large-scale production. This study addresses the classification of QDs synthesized in a tubular flow reactor consisting of a mixture of the desired InP/ZnS core−shell QDs and QDs made from the shell material, i.e., here ZnS QDs formed as a byproduct during the formation step of the ZnS shell. The homogeneous nucleation of ZnS nanoparticles from the shelling material introduces a heterogeneity in size and composition and affects the optical properties of the resulting QDs. To address this issue, we developed a size-selective agglomeration (SSA) technique by incrementally introducing ethanol as a poor solvent and classified the synthesized QDs into 13 distinct fractions. These 13 fractions are sorted into three distinct groups: (i) larger InP/ZnS QDs, (ii) a combination of smaller InP/ZnS QDs and larger ZnS QDs, and (iii) predominant ZnS QDs with some very tiny InP/ZnS QDs. The comprehensive characterization of the fractions was conducted using UV−visible absorption spectroscopy, photoluminescence spectroscopy, high-resolution scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy, total reflection X-ray fluorescence, and analytical ultracentrifugation. We could demonstrate that our method effectively separated unwanted ZnS QDs from the target InP/ZnS QDs. In addition, the fractions enriched in smaller InP/ZnS QDs exhibited a higher photoluminescence quantum yield compared to the fractions with larger QDs. This demonstrates the efficacy of SSA in finetuning the composition of QD mixtures produced on a larger scale to improve their functional properties. This approach provides fundamental understanding toward the development of a scalable two-dimensional classification process for such ultrasmall nanoparticles by particle size and composition