TY - JOUR A1 - Xu, Q. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Yang, Z. A1 - Wang, S. A1 - Gao, Y. A1 - Shang, J. A1 - Hunger, J. A1 - Aldiyarov, A. A1 - Schönhals, Andreas A1 - Ge, Y. A1 - Qi, Z. T1 - Molecular engineering of supramolecular polymer adhesive with confined water and a single crown ether N2 - Here, we report a water-induced supramolecular polymer built from confined structural water and an intrinsic amphiphilic macrocyclic self-assembly in a nanophase separated structure. The newly designed crown ether macrocycle, featuring strong hydrophilic hydrogen bonding receptor selenoxide and a synergistical hydrophobic selenium-substituted crown core, confines the structural water in a segregated, interdigitated architecture. Although water molecules typically freeze around 0 °C, the confined structural water in this supramolecular polymer remains in a liquid-like state down to 80 °C. Previous studies suggest that multiple crown ether units are needed to generate structural water. However, here, one unit is sufficient to control the formation and disappearance of structural water and consequent supramolecular polymerization. Typically, the DC conductivity of water shows Arrhenius temperature dependency (lnσDC ∝ 1/T). In contrast, this new crown unit maintains water in confined states, which exhibit a Vogel/Fulcher/Tammann behavior (lnσDC ∝ 1/(T-T0)) at temperatures above the glass transition temperature. Moreover, this water-induced supramolecular polymer exhibits remarkable adhesion properties to hydrophilic surfaces and maintains tough adhesion at low temperatures. These findings show how a single small macrocycle can govern the complex structure and functionality of water in supramolecular systems. KW - Supramolecular polymerization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623631 DO - https://doi.org/10.1039/D4SC06771A SN - 2041-6539 VL - 16 SP - 1 EP - 9 PB - RSC AN - OPUS4-62363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duarte Bernardino, Carolina A1 - Lee, Mihyun A1 - Ren, Qun A1 - Ruehle, Bastian T1 - Facile Spray-Coating of Antimicrobial Silica Nanoparticles for High-Touch Surface Protection N2 - The rising threat from infectious pathogens poses an ever-growing challenge. Metal-based nanomaterials have gained a great deal of attention as active components in antimicrobial coatings. Here, we report on the development of readily deployable, sprayable antimicrobial surface coatings for high-touch stainless steel surfaces that are ubiquitous in many healthcare facilities to combat the spread of pathogens. We synthesized mesoporous silica nanoparticles (MSNs) with different surface functional groups, namely, amine (MSN-NH2), carboxy (MSN-COOH), and thiol groups (MSN-SH). These were chosen specifically due to their high affinity to copper and silver ions, which were used as antimicrobial payloads and could be incorporated into the mesoporous structure through favorable host−guest interactions, allowing us to find the most favorable combinations to achieve antimicrobial efficacy against various microbes on dry or semidry high-touch surfaces. The antimicrobial MSNs were firmly immobilized on stainless steel through a simple two-step spray-coating process. First, the stainless steel surfaces are primed with sprayable polyelectrolyte solutions acting as adhesion layers, and then, the loaded nanoparticle dispersions are spray-coated on top. The employed polyelectrolytes were selected and functionalized specifically to adhere well to stainless steel substrates while at the same time being complementary to the MSN surface groups to enhance the adhesion, wettability, homogeneity, and stability of the coatings. The antimicrobial properties of the nanoparticle suspension and the coatings were tested against three commonly found pathogenic bacteria, Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli, as well as a fungal pathogen, Candida albicans. Especially MSN-SH loaded with silver ions showed excellent antimicrobial efficacy against all tested pathogens under application-relevant, (semi)dry conditions. The findings obtained here facilitate our understanding of the correlation between the surface properties, payloads, and antimicrobial activity and show a new pathway toward simple and easily deployable solutions to combat the spread of pathogens with the help of sprayable antimicrobial surface coatings. KW - Mesoporous silica nanoparticles KW - Thin films KW - Antimicrobial coatings KW - Spray-coating KW - Infectious diseases KW - Pathogen transmission KW - High-touch surfaces PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626269 DO - https://doi.org/10.1021/acsami.4c18916 SN - 1944-8252 SP - 1 EP - 13 PB - ACS Publications CY - Washington, DC AN - OPUS4-62626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Senbill, Haytham A1 - Gangan, Amr A1 - Saeed, Ahmed M. A1 - Gad, Mohammed E. A1 - Zeb, Jehan A1 - Fahmy, Alaa T1 - Effects of copper/graphene oxide core-shell nanoparticles on Rhipicephalus ticks and their detoxification enzymes N2 - Nanopesticides have been recently introduced as novel pesticides to overcome the drawbacks of using traditional synthetic pesticides. The present study evaluated the acaricidal activity of Copper/Graphene oxide core-shell nanoparticles against two tick species, Rhipicephalus rutilus and Rhipicephalus turanicus. The Copper/Graphene oxide core-shell nanoparticles were synthetized through the solution plasma (SP) method under different conditions. The nanoparticles synthesized at 180 W and 45 min were highly toxic to Rh. rutilus and Rh. turanicus, with 50% lethal concentration (LC50) values of 248.1 and 195.7 mg ml−1, respectively, followed by those which were synthesized at 120 W/30 mins (LC50 = 581.5 and 526.5 mg ml−1), 120 W/15 mins (LC50 = 606.9 and 686.7 mg ml−1), and 100/45 mins (LC50 = 792.9 and 710.7 mg ml−1), after 24 h of application. The enzyme assays revealed that 180 W/45 min treatment significantly inhibited the activity of acetylcholinesterase (115 ± 0.81 and 123 ± 0.33 U/ mg protein/min) and superoxide dismutase (290 ± 0.18 and 310 ± 0.92 U/ mg protein/min) in Rh. rutilus and Rh. turanicus, respectively, as compared with the negative control. The results also revealed a significantly increased catalase activity (895 ± 0.37 and 870 ± 0.31 U/ mg protein/min) in Rh. rutilus and Rh. turanicus, respectively. The above results indicated that Copper/Graphene oxide core-shell nanoparticles could be a promising alternatives for the management of ticks. KW - Copper/graphene oxide KW - Nanopesticides KW - Rhipicephalus rutilus KW - Rhipicephalus turanicus KW - Acetylcholinesterase KW - Antioxidants PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629359 DO - https://doi.org/10.1038/s41598-025-86560-4 SN - 2045-2322 VL - 15 SP - 1 EP - 12 PB - Springer Nature CY - London AN - OPUS4-62935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörmann, Anja Franziska T1 - GISAXS and XRR for STOP - M30 update N2 - With a representative set of samples measured in reflection geometry at the MOUSE we lead through our recent advances in this talk. A thin polystyrene film serves as an example for X-ray reflectivity and we show the effect of polishing on the reflectivity of stainless steel. Polystyrene spheres spin-coated onto different substrates including the polished stainless steel are demonstrated to show the characteristic scattering of spherical particles in GISAXS. We conclude with the first GISAXS data from laser-induced periodic surface structures (LIPSS) recorded at the MOUSE. T2 - M30 project meeting Surface Transfer of Pathogens (STOP) CY - Sofia, Bulgaria DA - 27.02.2025 KW - X-ray reflectivity KW - Substrate roughness KW - Grazing incidence KW - Particle-based coating PY - 2025 AN - OPUS4-62777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruehle, Bastian T1 - Natural language processing for automated workflow and knowledge graph generation in self-driving labs N2 - 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. KW - Natural Language Processing KW - Large Language Models KW - Self-Driving Labs KW - Materials Acceleration Platforms KW - Workflows KW - Nanomaterials KW - Advanced Materials PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631947 UR - https://github.com/BAMresearch/MAPz_at_BAM/tree/main/Minerva-Workflow-Generator DO - https://doi.org/10.1039/d5dd00063g SN - 2635-098X SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zaki, Mohammad T1 - Nano- And Advanced Materials Synthesis In A Self-driving Lab (SDL) N2 - Development of new nano- and advanced materials - or improvement of existing ones - are important drivers in materials research due to the high importance of these material classes for various applications. Traditional laboratory methods for material development often suffer from reproducibility issues, inefficiencies, human errors, and long experimental optimization times. To overcome these challenges and thus accelerate and optimize the process of material synthesis and discovery, we are building a Self-Driving Lab (SDL), in which we integrate robotics for autonomous nanomaterial synthesis, and automated characterization and data analysis for a complete and reliable nanomaterial synthesis workflow. We also leverage artificial intelligence (AI) and machine learning (ML) algorithms to analyze characterization results and plan new experiments to optimize material properties in an ML-guided active learning feedback loop. Our SDL is very agnostic towards the types of nano- and advanced materials it can synthesize. On the same SDL platform, we successfully synthesized Stober silica, mesoporous silica, copper-oxide, and gold nanoparticles, as well as metal-organic frameworks and more complex structures from multi-step reactions, such as Au@SiO2 and CuO@SiO2 core-shell nanoparticles. All these material syntheses showed excellent reproducibility when run on the SDL platform multiple times. Automated, in-line characterization measurements of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence) of the nanomaterials have also been incorporated in the SDL, along with automating data analysis of at-line or off-line characterization techniques such as electron microscopy image analyses [1]. Incorporating these characterization results alongside a machine learning feedback loop that suggests new experimental parameters for obtaining materials with target properties is a key step for developing autonomous, closed-loop optimization processes. In such a process, we typically start by using random sampling to suggest initial experimental parameters, followed by ML-guided active learning algorithms such as Bayesian optimization, artificial neural networks, or downhill simplex optimizers (e.g., Nelder-Mead) that suggest new synthesis parameters to finally arrive at a material with the targeted or enhanced properties. Further improvement and optimization of our SDL has the potential to mitigate challenges faced by traditional approaches and open a way for rapid and reproducible nano- and advanced material synthesis, optimization, and discovery. T2 - ANAKON Conference 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Self-driving laboratories KW - Materials acceleration platforms KW - Nanomaterials KW - Advanced materials KW - Automation KW - Robotics KW - In-line characterization PY - 2025 AN - OPUS4-62737 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schoenhals, Andreas T1 - The bahvior of inonic liquid crystals as investigated by broadband dielectric spectroscopy and complementary methodas N2 - The behavior of liquid crystals based on phenylbenzoate was investigated using broadband dielectric spectroscopy and advanced calorimetry. The length of the alkyl side chain was systematically varied from 8 to 16 carbon atoms. The experimental results were compared with those obtained from molecular dynamics simulations. T2 - Sympoium: "Dipoles is soft matter - How they move and organize" CY - Leuven, Belgium DA - 06.06.2025 KW - Ionic liquid crystals PY - 2025 AN - OPUS4-63316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Juranyi, F. A1 - Kruteva, M. A1 - Zorn, R. A1 - Schönhals, Andreas T1 - Low-Frequency Vibrational Density of States of Nanophase- Separated Poly(n‑alkyl methacrylate)s: Confined Phonons and Relationship to Specific Heat N2 - This study investigates the low-frequency vibrational Density of states of nanophase-separated poly(n-alkyl methacrylate)s (PnMAs) and its relationship to specific heat. This system undergoes a nanophase separation for n > 1 in alkyl side chain-rich domains and a backbone-rich matrix. Using inelastic neutron scattering, the low-frequency vibrational density of states (Boson peak, BP) of PnMAs with varying alkyl side chain lengths (methyl, butyl, hexyl, and octyl) is measured. The results reveal that the BP shifts to higher frequencies with increasing side chain length reaching a maximum. This result indicates a counterbalance of confinement effects and the scattering of the matrix. The behavior of the Boson peak of the PnMAs is compared to other nanophase-separated systems, such as Janus-polynorbornenes and hexakis(n-alkyloxy)triphenylene discotic liquid crystals. The study also explores the connection between the BP and specific heat capacity, showing a linear relationship between the maximum frequency of the BP and the maximum temperature of the specific heat capacity anomaly. Moreover, from the measured vibrational density of states, the specific heat capacity is calculated and compared to experimental results. The comparison reveals qualitative agreement between the calculated and experimental data. These findings provide evidence for the sound wave interpretation of the Boson peak. KW - Inelastic Neutron Scattering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636928 DO - https://doi.org/10.1021/acs.macromol.5c00898 SN - 1520-5835 SP - 1 EP - 12 PB - ACS Publications AN - OPUS4-63692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawek, Marcel A1 - Szymoniak, Paulina A1 - Hülagü, Deniz A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Molecular Mobility of Thin Films and the Adsorbed Layer of Poly(2-vinylpyridine) N2 - The molecular dynamics of thin films and the adsorbed layer of poly(2-vinylpyridine) (P2VP) were investigated using broadband dielectric spectroscopy (BDS) and spectroscopic ellipsometry. Thin films of P2VP were prepared on silicon substrates and characterized to understand the influence of film thickness on the thermal glass transition temperature (Tg) and molecular mobility. The ellipsometric study revealed a decrease in Tg with decreasing film thickness, attributed to the enhanced mobility at the polymer/air interface. The adsorbed layer, prepared via the solvent leaching approach, exhibited a higher Tg compared to the bulk, indicating reduced molecular mobility due to strong polymer substrate interactions. The dielectric measurements were carried out in two different electrode configurations, crossed electrode capacitors (CEC) and nanostructured electrodes (NSE), where the latter allows for a free surface layer at the polymer/air interface. The relaxation rates of the α-relaxation measured in the CEC geometry collapse into one chart independent from the film thickness. For the thin films measured in the NSE arrangement the relaxation rates slow down with decreasing film thickness which was discussed as related to a stronger interaction of the P2VP segments with the native SiO2 at the surface of the silicon substrate compared to aluminum. It is worth to note that the effect of the enhanced mobility at the polymer/air interface is not observed in the dielectric measurements. BDS measurements in NSE geometry identified an additional relaxation process (α*-relaxation) in thin films, which was more pronounced in the adsorbed layer. This process is hypothesized to be related to molecular fluctuations within the adsorbed layer including the adsorption/desorption dynamics of segments or to a Slow Arrhenius Process (SAP) related to the equilibration dynamics deep in the glassy state. KW - Thin polymer films PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637181 DO - https://doi.org/10.1039/d5sm00539f SN - 1744-6848 SP - 1 EP - 12 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Böhning, Martin A1 - De Souza, N. R. A1 - Juranyi, F. A1 - Zorn, R. A1 - Schönhals, Andreas T1 - Inelastic and Quasielastic Neutron Scattering on Polynorbornenes with Bulky Carbocyclic Side groups N2 - This study investigates the molecular mobility and vibrational properties of polynorbornenes with bulky carbocyclic side groups using inelastic and quasielastic neutron scattering techniques. The polymers, synthesized via metathesis and addition polymerization, exhibit varying degrees of microporosity, which ignificantly influences their gas separation performance. By inelastic neutron scattering experiments, it could be shown that all considered polymers have excess contributions to the low frequency vibrational density of states known as the Boson peak. The maximum frequency of the Boson peak correlates to the microporosity of the polymers. This correlation supports the sound wave interpretation of the Boson peak, suggesting that the microporous structure enhances the compressibility of the material at a microscopic length scale. The molecular mobility, particularly the methyl group rotation, was characterized using elastic scans and quasielastic neutron scattering. The study revealed a temperature dependent relaxation process, with the onset of molecular fluctuations observed around 200 K for the polymer containing methyl groups. For the polymer having no methyl groups only elastic scattering is observed. The methyl group rotation was analyzed in terms of a jump diffusion in a threefold potential with three equivalent energy minima. This leads to an almost correct description of the q dependence of the elastic incoherent scattering function when the number of hydrogen nuclei undergoing the methyl group rotation is considered. It was further evidenced that the fraction of methyl undergoing the methyl group rotation increases with increasing temperature. KW - Polymers of Intrinsic Microporosity KW - Neutron scattering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630297 DO - https://doi.org/10.1016/j.polymer.2025.128358 SN - 1873-2291 VL - 328 SP - 241 PB - Elsevier Ltd. AN - OPUS4-63029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stühler, Merlin R. A1 - Makki, Hesam A1 - Silbernagl, Dorothee A1 - Dimde, Mathias A1 - Ludwig, Kai A1 - Tegner, Bengt E. A1 - Greve, Christopher A1 - Rausch, Konstantin A1 - Herzig, Eva M. A1 - Köhler, Anna A1 - Plajer, Alex J. T1 - Flexibility and Dynamicity Enhances and Controls Supramolecular Self-Assembly of Zinc(II) Metallogels N2 - Supramolecular self-assembly of stacked architectures is typically achieved through hydrogen bonding or π–π interactions between monomers constructed from stable and inert bonds. In contrast, coordinative interactions of early metals promise distinct self-assembly behaviour due to more flexible bonding geometries and a wider range of stabilities and exchange kinetics. In this report we demonstrate that tailoring the flexible coordination sphere of Zinc(II) complexes via subtle ligand modification promotes not only one but also three-dimensional self-assembly both thermodynamically and kinetically into higher-order fibrous morphologies, the latter being elucidated by electron tomography. As a result, coordination chemistry can be translated into both nanoscopic (fibre stiffness) and macroscopic (thermal gel stability) material properties. Utilizing dynamicity enables gelation via subcomponent self-assembly, constructing the supramolecular polymer network simultaneously with the monomer. Furthermore, coordinative dis- and reassembly via metal-ligand exchange reactions involving the first and second coordination spheres allows for control over gelation and emission of the system. Our report links concepts in supramolecular self-assembly and coordination chemistry by leveraging the unique bonding interactions that cannot be achieved for traditional monomers, promising applications in stimuli-responsive optoelectronics. KW - Nanomaterial KW - AFM KW - Organometallic KW - Gel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634221 DO - https://doi.org/10.1002/adfm.202507793 SN - 1616-301X SP - 1 EP - 10 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-63422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörmann, Anja Franziska T1 - My surface at a glance: grazing incidence scattering applications N2 - Three literature examples are presented to demonstrate the wide range of applications of grazing incidence scattering. These examples concern 1) the determination of the density of a porous film, 2) how orientation of conducting polymers is observed in grazing incidence scattering, and 3) how the three-dimensional order of nanoparticles is reflected in the data. To conclude we show recent data from the MOUSE lab demonstrating the new capability to observe intermolecular distances in thin films using the molybdenum X-ray source. T2 - Surface Transfer of Pathogens (STOP) - M37 meeting CY - Turin, Italy DA - 11.09.2025 KW - Grazing incidence KW - GISAXS KW - Applications PY - 2025 AN - OPUS4-64115 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hussein, S. A1 - Kühl, A. A. A1 - Golusda, L. A1 - Plattner, C. A1 - Heinze, N. A1 - Sturm, G. A1 - Freise, C. A1 - Traub, Heike A1 - Schannor, Mathias A1 - Trajanoski, Z. A1 - Taupitz, M. A1 - Siegmund, B. A1 - Paclik, D. T1 - Phenotype and function of human monocytes remain mainly unaffected by very small superparamagnetic iron oxide particles N2 - The field of medical application of organic or inorganic nanoparticles is extensive. Medical nanoparticles offer benefits but pose risks. For safe use in diagnostics and therapy, they should be inert, non-immunogenic, non-aggregating, and avoid long-term accumulation in sensitive tissues like bone marrow or the brain. We have developed in-house very small superparamagnetic iron oxide nanoparticles (VSOP), 7 nm in size, which have been successfully used in preclinical magnetic resonance imaging (MRI) to detect intestinal inflammation, neuroinflammation and atherosclerosis. This study examines nanoparticle effects on human blood cells focusing on monocytes in vitro as a first step toward clinical application. Whole blood and monocytes from healthy donors and patients with inflammatory bowel disease were treated with VSOP in vitro and analyzed for changes in their transcriptome, phenotype and function. RNA sequencing of monocytes identified the transferrin receptor as one of the most significantly downregulated genes after VSOP treatment, likely to limit iron uptake. Whereas whole blood RNA sequencing showed significant changes only in three non-coding genes. CyTOF analysis confirmed that VSOP-treated monocytes remain inactive, with no increased proliferation or altered migration. Metabolically, VSOP uptake enhanced the oxygen consumption rate. This effect was likely due to phagocytosis rather than effects mediated by the VSOP itself, as phagocytosis of latex beads showed comparable results. In summary, the analysis of peripheral blood mononuclear cells and monocytes suggests that VSOP treatment has no major impact on immune cell phenotype or function indicating VSOP as a promising diagnostic tool in MRI for inflammatory bowel disease. KW - Imaging KW - Nanoparticle KW - Monocytes KW - Contrast agent KW - Diagnostics KW - ICP-MS KW - LA-ICP-MS KW - VSOP PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632012 DO - https://doi.org/10.3389/fnano.2025.1584000 SN - 2673-3013 VL - 7 SP - 1 EP - 16 PB - Frontiers Media CY - Lausanne AN - OPUS4-63201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz A1 - Ermilova, Elena A1 - Weise, Matthias A1 - de Préville, Sophie A1 - Hoffmann, Johannes A1 - Morán-Meza, José A1 - Piquemal, Francois A1 - Hertwig, Andreas T1 - Characterization of electrical properties in microstructured ITO layers using spectroscopic ellipsometry N2 - Thin indium tin oxide (ITO) layers are essential in optoelectronics due to their good electrical conductivity, optical transparency in the visible and near infrared regions, substrate adherence and chemical stability. They are widely used in photovoltaic cells, displays, and organic LEDs, and as low emissivity coatings in smart windows and energy-efficient buildings. For nanophotonic devices, understanding the interplay of ITO’s optical and electrical properties is crucial. Electrical resistivity can be tuned by modifying deposition conditions and layer thickness. However, measuring these properties, especially on microstructured surfaces, remains challenging due to the issues like homogeneity and instability during etching. Spectroscopic ellipsometry (SE), a non-destructive and phase-sensitive optical technique, offers precise measurement of thin film thickness and dielectric properties. In this study, we investigated the layer thickness, optical constants, and sheet resistance of unstructured and microstructured ITO thin layers using SE. Unstructured layers were deposited via DC-magnetron sputtering on silicon (Si) substrates in argon (Ar) atmospheres with varying oxygen (O2) flows. This multi-technique approach enhances the understanding of ITO layer structuring and provides robust methodologies for correlating optical and electrical properties, advancing metrology for nanotechnology applications and material science. It also opens the pathway to new reference samples and calibration methods for electrical properties involving device-like structured samples. T2 - ICSE10 - 10th International Conference on Spectroscopic Ellipsometry CY - Boulder, CO, USA DA - 08.06.2025 KW - Ellipsometry KW - Indium tin oxide (ITO) KW - Scanning microwave microscopy (SMM) KW - Sheet resistance calibration standards KW - ITO wet etching PY - 2025 AN - OPUS4-63631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data acquisition system for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution N2 - This study presents our data acquisition system prototype for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution (nanoDAQ) and a matching data processing approach for time-resolved data in the nanosecond range. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. Particle-by-particle-based analysis of ion event density and other parameters derived from nanosecond time resolution show promising results. High data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leaves only the sample uptake and rinsing steps as remaining factors for limiting the total measurement time. T2 - 20th European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization PY - 2025 AN - OPUS4-63599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Speight, Isaiah R. A1 - Ardila-Fierro, Karen J. A1 - Hernández, José G. A1 - Emmerling, Franziska A1 - Michalchuk, Adam A. L. A1 - García, Felipe A1 - Colacino, Evelina A1 - Mack, James T1 - Ball milling for mechanochemical reactions N2 - Mechanochemistry is an emerging field with the potential to pave the way for sustainable chemistry. Although the use of mechanical force to initiate chemical reactions has been recognized for millennia, it has often taken a backseat to thermal and photonic methods. Over the past 30 years, mechanochemistry has seen a resurgence of interest, attracting researchers across the globe. Despite its proven ability to address numerous challenges within the chemical community, mechanochemistry remains on the periphery. This Primer serves as a valuable guide for conducting mechanochemical reactions by ball milling, offering an overview of the processes, methods, tools and terminology necessary to embark on research in this field. It also highlights persistent hurdles such as equipment standardization, understanding the impact of new discoveries and the lack of predictability of reaction outcomes. The Primer’s focus is on how mechanochemical ball milling is used in various chemical transformations, distinguishing it from other forms of mechanochemistry discussed in the literature. With a promising future, this Primer serves as a gateway for those aspiring to contribute to the field’s advancement. KW - Mechanochemistry KW - Ball milling KW - Upscaling PY - 2025 DO - https://doi.org/10.1038/s43586-025-00401-2 SN - 2662-8449 VL - 5 IS - 1 SP - 1 EP - 18 PB - Springer Science and Business Media LLC AN - OPUS4-63447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenbusch, Ivo A1 - Arai, Marylyn Setsuko A1 - Rizzo, Fabio A1 - de Camargo, Andrea S. S. A1 - Ravoo, Bart Jan T1 - A host–guest approach to ratiometric pH sensing using upconversion nanoparticles N2 - A new pH nanosensor based on β-NaYF4:Yb3+/Tm3+ upconversion nanoparticles functionalized with cyclodextrin and a pH-sensitive adamantane-modified nitrobenzoxadiazole dye (NBD-Ad). KW - Host-guest materials KW - Upconversion nanoparticles KW - Ratiometric optical sensors KW - pH sensing PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637722 DO - https://doi.org/10.1039/d5na00145e SN - 2516-0230 VL - 7 IS - 13 SP - 4142 EP - 4151 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Go, Eun Sul A1 - Hong, Eun Ji A1 - Lee, Ji Yeong A1 - Stolar, Tomislav A1 - Peterson, Gregory I. A1 - Emmerling, Franziska L. A1 - Kim, Kyoungsoo A1 - Kim, Jeung Gon T1 - Insights into Mechanochemical Solid-State Ball-Milling Reaction: Monitoring Transition from Heterogeneous to Homogeneous Conditions N2 - As mechanochemical synthesis has advanced significantly, there has been intense interest in understanding the underlying mechanisms of these reactions. Given that many mechanochemical processes are conducted in the solid-state without solvation yet sometimes yield faster reactions than those in solution, we sought to address the following question: Are mechanochemical reactions homo- or heterogeneous? To investigate, we employed a model system involving the mixing and copolymerization of l-lactide (LLA) and d-lactide (DLA), monitored through powder X-ray diffraction (PXRD), nuclear magnetic resonance, and differential scanning calorimetry. In situ and ex situ PXRD analyses of the mixture of LLA and DLA showed that vibratory ball milling rapidly transformed the initially heterogeneous lactide mixture into a homogeneous phase within one min due to collisions between the balls and the jar. By varying the milling conditions, we were able to regulate the level of mixing, which subsequently influenced the copolymerization outcomes. In the solid-state ball-milling copolymerization of LLA and DLA in the presence of a catalyst and initiator, multiblock copolymers of poly(l-lactic acid) and poly(d-lactic acid) were formed within one min during the early stage of the reaction, when incomplete mixing of the monomers led to a process governed by phase heterogeneity. In contrast, prolonged polymerization promoted conditions approaching homogeneity, ultimately yielding atactic poly(lactic acid). This transition from heterogeneous to homogeneous reactions is a distinctive feature compared to conventional homogeneous reactions, potentially leading to mechano-exclusive reaction designs. KW - Mechanochemistry KW - Ball-milling KW - Homogeneous reaction KW - Heterogeneous reaction PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638008 DO - https://doi.org/10.1021/jacsau.5c00322 SN - 2691-3704 VL - 5 IS - 6 SP - 2720 EP - 2727 PB - American Chemical Society (ACS) AN - OPUS4-63800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deffo, Gullit A1 - Tamo, Arnaud Kamdem A1 - Fotsop, Cyrille Ghislain A1 - Tchoumi, Honorine Hortense Bougna A1 - Talla, Donald Eric Njiajo A1 - Wabo, Calice Gildas A1 - Deussi, Marcel Cédric Ngaha A1 - Temgoua, Ranil Clément Tonleu A1 - Doungmo, Giscard A1 - Njanja, Evangeline A1 - Tonle, Ignas Kenfack A1 - Puzari, Panchanan A1 - Birkemeyer, Claudia A1 - Ngameni, Emmanuel T1 - Metal-organic framework-based materials: From synthesis and characterization routes to electrochemical sensing applications N2 - Metal-organic frameworks (MOFs) are formed by coordination bonds between organic ligands and metal ions or clusters. Their key properties, including high surface area, porosity, and adjustable functionalities, enable diverse applications in gas separation, catalysis, energy storage, luminescence, and more recently, the development of electrochemical sensors. In this review, we provide an overview of various electrochemical methods and discuss different MOF-based electrochemical sensors reported in the literature. We focus on the synthesis of MOFs, their characterization, and the preparation of MOF-based working electrodes for electroanalysis. A brief history of MOFs, along with their nomenclature, classifications, and features, is discussed to provide a chronological understanding of MOFs before delving into their electroanalytical uses. Recent advancements in the use of MOFs as electrode materials for electrochemical sensing have been extensively reviewed and documented, highlighting their increasing relevance in various analytical fields. This review investigates the key properties of MOFs that make them suitable candidates for sensing applications and the ability for post-synthesis modifications to improve their selectivity and sensitivity. It also examines the challenges associated with the synthesis and modification of MOFs, including issues related to scalability, eproducibility, and the stability of the materials under operational conditions. Furthermore, the review discusses potential future directions for the use of MOFs in electrochemical sensing, emphasizing their role as electrode materials to enhance the sensitivity and selectivity of modified sensors for sustainable applications. KW - Metal-organic frameworks (MOFs) KW - MOF synthesis and characterization KW - Electrochemical sensors KW - Electroanalysis PY - 2025 DO - https://doi.org/10.1016/j.ccr.2025.216680 SN - 0010-8545 VL - 536 SP - 1 EP - 78 PB - Elsevier B.V. AN - OPUS4-63742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - Workflow generation, management, and semantic description for Self-Driving Labs N2 - The software backend that controls the robotic hardware and runs the synthesis workflows is a very important component of any Self-Driving Lab (SDL). On the one hand, it has to deal with orchestrating and managing complex and task-specific hardware through low-level communication protocols and plan and use the available resources as efficiently as possible while executing (parallelized) workflows, on the other hand, it is the interface the users use to communicate with this highly complex platform, and as such, it needs to be as helpful and user-friendly as possible. This includes the AI-aided experimental design in which the system helps the user to decide which experiment to run next, providing automated data analysis from characterization measurements, and offering easy to understand tools and graphical user interfaces for generating the workflows that are executed on the platform. Lastly, the specificity of the workflows and their dependence on the hardware and software of the SDLs necessitates a common description or ontology for making them easily interchangeable and interoperable between different platforms and labs. In this contribution, we present several key aspects of “Minerva-OS”, the central backend that orchestrates the syntheses workflows of our SDL for Nano- and Advanced Materials Syntheses [1]. One key feature is the resource management or “traffic control” for scheduling and executing parallel reactions in a multi-threaded environment. Another is the interface with data analysis algorithms from in-line, at-line, and off-line measurements. Here, we will give examples of how automatic image segmentation of electron microscopy images with the help of AI [2] can be used for reducing the “data analysis bottleneck” from an off-line measurement. We will also discuss, compare, and show benchmarks of various machine learning (ML) algorithms that are currently implemented in the backend and can be used for ML-guided, closed-loop material optimization in our SDL. Lastly, we will show our recent efforts [3] in making the workflow generation on SDLs more user-friendly by using large language models to generate executable workflows automatically from synthesis procedures given in natural language and user-friendly graphical user interfaces based on node editors that also allow for knowledge graph extraction from the workflows. In this context, we are currently also working on an ontology for representing the process steps of the workflows, which will greatly facilitate the semantic description and interoperability of workflows between different SDL hardware and software platforms. T2 - Accelerate 2025 CY - Toronto, Canada DA - 11.08.2025 KW - Nanomaterials KW - Advanced Materials KW - Workflows KW - Machine Learning KW - SDL PY - 2025 AN - OPUS4-63936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -