TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Salzmann, Christoph A1 - Pellegrino, F. A1 - Durand, B. A1 - Taché, O. A1 - Zurutuza, A. T1 - Role of Sample Preparation for Accurate and Automated Morphological Analysis of Nanoparticles proven in Interlaboratory Comparison Exercises N2 - Traceable morphological and chemical characterization of nanomaterials with respect to the various possible sizes, size distributions, shapes, and concentrations of real-world nanoparticles (NPs) is a challenging task. Particularly for the nonspherical, non-monodisperse nanoparticles – as typically for most of the commercial particles, including their strong tendency to agglomerate, there is a lack of standard operation procedures providing accurate nanoparticle characterisation. In the framework of the pre-standardisation framework of VAMAS (Versailles Project on Advanced Materials and Standards, www.vamas.org) two interlaboratory comparison (ILC) studies are being carried out under the Technical Working Area (TWA) 34 “Nanoparticle Populations”:i) Project #15 addresses the analysis of the size and shape distribution of TiO2 bipyramidal NPs by traceable imaging methods such as TEM, SEM, STEM-in-SEM, AFM as well as with SAXS as an ensemble method. This ILC is thought as the next level development of the case studies exemplified in the published ISO standards ISO 21363 and ISO 19749. It was agreed to complete the first ILC with the NPs already prepared according to the same procedure on a TEM grid, and, at a later stage, to carry out second ILCs with the same NPs distributed to the participants as liquid suspensions together with protocols for the uniform NP deposition on suited substrates - as developed and optimized within the European project nPSize. Once having good deposition protocols available, the door for automated image analysis gets opened. Corresponding image analysis protocols and reporting templates have been distributed to the ILC participants, too. ii) Project #16: two spherical SiO2 NP samples with bi-modal size distributions in two nominal relative number concentrations were prepared and distributed also as liquid suspensions accompanied by sample preparation, measurement, and image analysis protocols and reporting templates. Here, the NP concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations (relative populations of the two modes). The results of all the participating laboratories, in both ILCs, compiled in comparative representations will be shown and discussed for the first time. The reduction of the measurement uncertainties associated to the size, shape and number-concentration results induced by the significant improvement of the sample preparation on substrates (as single particles with a high-density coverage), combined with welldefined image analysis procedures will be highlighted. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Nanoparticles KW - VAMAS KW - Interlaboratory comparison KW - Sample preparation KW - Nanoparticle concentration PY - 2024 AN - OPUS4-60453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Sachse, René A1 - Matjacic, L. A1 - McMahon, G. A1 - Bernicke, M. A1 - Bernsmeier, D. A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Chemical Nanoscale Analysis of Mesoporous Mixed IrOx-TiOx Thin Films N2 - Porous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach. Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too. In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Thin films KW - Mesoporous KW - IR oxide KW - Ti oxide KW - Porosity PY - 2024 AN - OPUS4-60452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matthews, Lauren A1 - Sahre, Mario A1 - Hesse, R. A1 - Schusterbauer, Robert A1 - Grant, M. A1 - Agudo Jacome, Leonardo A1 - Albrecht, T. A1 - Hodoroaba, Vasile-Dan T1 - Approaches to Surface Analysis of Modified Quartz Nanopipettes N2 - Nanopipettes are a type of solid-state nanopore with needle-like geometry. Their applications range from imaging, sensing, diagnostics, and use as injectors. The response of nanopipette sensors is highly dependent on the size, geometry and chemical properties of the sensing region. As nanopipettes are increasingly tuned and modified for specific analytes, a better understanding of the surface chemistry and morphology of the inner channel is necessary. For exploring these effects, quartz nanopipettes were modified by gas phase silanization, a well-utilised technique in the field to enhance performance of nanopipettes, and further functionalised with a metal bis thiolate complex, to aid in chemical analysis. The inner channel of the sensing region was exposed with focused ion beam (FIB) milling as a dedicated sample preparation method for nanoscale surface analysis. The sample characterisation involved scanning electron microscopy (SEM), Auger electron spectroscopy (AES) and low-energy energy dispersive x-ray spectroscopy (EDX). The results demonstrate the first steps towards full characterisation of nanopipettes at the nanoscale, notably with access to the inner channel. The methods used here can be applied to gain further understanding of the response of these sensors to complex analytes, and allow for the study of different surface functionalisation at the all-important sensing region. T2 - 2024 Spring Meeting of the European Materials Research Society (E-MRS) CY - Strasbourg, France DA - 27.05.2024 KW - Nanopipettes KW - FIB KW - Surface analysis KW - Surface modification KW - Silanisation PY - 2024 AN - OPUS4-60449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of Lateral Dimensions of Particles & Flakes (2D) by Imaging Methods N2 - An overview with the basics of size and shape measurement of particles and 2D structures according to established methodologies (and popular imaging processing software packages) with imaging techniques is given. Main descriptors are explained based on practical cases are determined interactively at the flipchart. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Nanoparticles KW - 2D materials KW - Lateral dimensions KW - ISO KW - Imaging PY - 2024 AN - OPUS4-60454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matthews, Lauren T1 - Rapid Desease Monitoring with Resistive-Pulse Sensing in Nanopipettes N2 - Following parts of the research project as proceeded at University of Birminngham are presented: Translocation, Experiments, Synthesis of DNA Structures, Antibody, Biomarker, Binding. Following works have been carried out at BAM: High Resolution Electron Microscopy, Dedicated Sample Preparation, Surface Analysis Methods. T2 - UoB-BAM Chemistry Theme Meeting CY - Online meeting DA - 15.05.2024 KW - Nanopipettes KW - Sensing KW - Diagnosis KW - Surface analysis PY - 2024 AN - OPUS4-60451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Chemello, Giovanni A1 - Reed, B.P. A1 - Marchesini, S. A1 - Pollard, A.J. A1 - Clifford, C.A. T1 - Reliable measurements of the chemical composition of graphene-related 2D materials with X-ray photoelectron spectroscopy N2 - Graphene and related 2D materials (GR2Ms) are now entering an exciting phase of commercialization and use in products. Graphene nanoplatelets (GNPs) can be obtained in rather large quantities, but the properties of these industrially produced powders can vary depending on the production method, and even from batch to batch. Understanding and optimizing the surface chemistry of GNPs, modified through chemical functionalization processes is crucial, because it affects their dispersibility in solvents and matrices for the purpose of embedding them into real-world products. Therefore, reliable and repeatable measurements of the surface chemistry of functionalized GNPs are an important issue for suppliers as well as users of these materials. To address these concerns, international documentary ISO standards for measurement methodologies are under development which incorporate protocols that are becoming widely accepted in the community. Recently, it was shown that pelletizing led to lower average O/C atomic ratios than those measured for powders [1]. In another study, the influence of the morphology on the degree of functionalization was shown [2]. As expected, a higher degree of functionalization was detected for smaller GNPs. The functionalization was located at the outermost surfaces of the GNPs by comparing experiments using photoelectron with soft (Al Kα, 1.486 keV) and hard X-rays (Cr Kα, 5.405 keV). Therefore, it is important for those using GNPs to understand both the physical and chemical properties of these particles, when considering their use in different applications. The next step for reliable characterization protocols was the realization of an interlaboratory comparison under the auspices of VAMAS (Versailles Project on Advanced Materials and Standards) with 22 participating laboratories from all over the world. Samples of oxygen-, nitrogen-, and fluorine- functionalized GNPs were provided to the participants along with a measurement protocol. Participants were asked to prepare the samples as powders on a tape, powders in a sample holder recess, or as pellets. The lower measured O/C ratio reported for pelletized samples [1] was confirmed. The lowest scattering of the results was observed for the powders measured in the recess (Fig. 1). Furthermore, an influence of the humidity on the results was observed. T2 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - Interlaboratory Comparison KW - Functionalized graphene KW - Sample preparation PY - 2024 AN - OPUS4-60533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Ciornii, Dmitri A1 - Knigge, Xenia A1 - Hodoroaba, Vasile-Dan A1 - Bennet, F. A1 - Meirer, F. A1 - Duijndam, A. A1 - Thünemann, Andreas A1 - Drexel, R. A1 - Fadda, M. A1 - Sacco, A. A1 - Giovannozzi, A.M. A1 - Donskyi, I. A1 - Schusterbauer, R. A1 - Nickl, P. A1 - Reichardt, P. A1 - Altmann, Korinna T1 - Revealing surface functionalities of micro- and nanoplastic particles’ surface by means of XPS N2 - Over the last 20 years, many researchers, politicians, and citizens themselves have become increasingly aware of the growing plastic problem of our time. Inadequate recycling concepts, collection points, and careless dumping of plastic products in the environment lead to an accumulation of plastic. External weather influences can cause these to degrade and fractionate, so that today microplastics (1-1000 µm, ISO/TR 21960:2020) [1] of different polymer materials can be detected in all parts of the world. The precautionary principle applies to microplastics. The particles can break down further to form nanoplastics (<1 µm, ISO/TR 21960:2020) [1]. Whether microplastics or nanoplastics pose a toxicological hazard is being investigated in a variety of ways. Valid results are still pending, however, investigations into the frequency, transport, possible sinks and entry paths must be taken into account. This is why monitoring of microplastics is already required in the revision of the Drinking Water Framework Directive [2]. The same is still pending in the final version of the revision of the Waste Water Framework Directive this year, but is expected. Nanoplastics are particularly under discussion for having a toxic effect on humans and animals, as these particles are small enough to be absorbed by cells. For targeted toxicological studies, it is important to have test and reference materials that resemble the particles found in the environment. To mimic environmental samples, these materials should also have an irregular shape and show aging at the surface, which can be detected with XPS or SEM/EDS. BAM in collaboration with the EMPIR project "PlasticTrace" works on a reference material candidate of nano-sized polypropylene (nano-PP) [3]. The nano-PP vials were tested for homogeneity with PTA and further characterized with bulk and surface-sensitive techniques. An SEM image and a corresponding XPS spectrum are presented in Figure 1. Raman measurements as well as XPS indicate an aged surface. T2 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - Surface chemistry KW - Micro- and nanoplastics KW - X-ray Photoelectron Spectroscopy KW - MNP production technique PY - 2024 AN - OPUS4-60535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Weimann, T. A1 - Bütefisch, S. T1 - A new XPS test material for more reliable surface analysis of microstructures N2 - Small-area XPS analysis is one of the most popular and powerful methods for analysing the surface of features in the micro-range. When measuring microstructures, the ques-tion arises whether the measuring point is really located at the point intended to be ana-lysed. Information in a measured spectrum might originate within the field of view (FoV) on the surface of the sample, from outside the FoV, or even from inherent contamination. To ensure that small structures can be measured correctly regardless of user and instru-ment, certain instrument and sample settings must be known and selected correctly: beam and aperture size as well as the aperture settings and the approximate dimensions of the structure to be analysed. This is the only way to ensure that the information in the spectrum originates only from the FoV on the analysed structure. To test the performance of the XPS instruments, a dedicated test material was developed that consists of a gold surface on which 8 circles and 8 squares of chrome are incorpo-rated using a masking process, so that the Au substrate and the Cr structure surfaces are in the same surface plane. In order to be able to test as many as possible instruments from different manufacturers, the structures have been designed with a size ranging from 300 µm down to 7 µm. The layout of the test material has been optimised in regard of the handling. The structures are arranged along lines instead of a circumference, marking arrows around the smaller structures (≤50 µm) are added, and the lithography mask is optimised regarding edge and diffraction effects. Furthermore, the manufacturing process was changed from electron-beam deposition to mask lithography due to costs reasons. The structures on the test material were measured with a metrological SEM to determine their accurate dimensions and check the repeatability of the manufacturing process. XPS investigations with a Kratos AXIS Ultra DLD and an ULVAC-Phi Quantes demonstrates the suitability of this new test material for measuring the analysed area. T2 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - Small-area XPS KW - Test material KW - Field of view KW - Imaging PY - 2024 AN - OPUS4-60539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Favre, G. T1 - How to expand the use of your test method? Validation is key towards standardisation N2 - Standardised methods need validation. The main validation parameters like trueness, repeatability and intermediate precision and reproducibility are presented. Furthermore, different methods for the validation are disussed: (certified) reference materials, representative testing materials and interlaboratory comparisons. At last, the need of proficiency testing is stressed. T2 - Materials Week 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Validation KW - Reproducibility crisis KW - Metrological traceability KW - Measurement uncertainty PY - 2024 AN - OPUS4-60536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Habibimarkani, Heydar A1 - Abram, Sarah Luise A1 - Prinz, Carsten A1 - Hodoroaba, Vasile-Dan T1 - Comparative chemical analysis of Ni-Fe oxide nanoparticles N2 - Ni-Fe oxide nanoparticles have gained a lot of interest because of their high activity in the oxygen evolution reaction (OER) which is crucial for water splitting. [1] Although there have been great efforts in the last years, the understanding of the synergistic effect between Fe and Ni is still under discussion. Therefore, we prepared different Ni-Fe oxide nanoparticles with different compositions from pure iron oxide to pure nickel oxide adapting a known procedure. [2,3] Size and morphology of the nanoparticles depend on the composition which was shown with Transmission Electron Microscopy (TEM). The compositions of the nanoparticles were measured with a comparative approach using X-ray Photoelectron Spectroscopy (XPS), Hard X-ray Photoelectron Spectroscopy (HAXPES), and Energy Dispersive X-Ray Spectroscopy (EDS) coupled with the TEM providing detailed chemical information of the nanoparticles in different sample regions. EDS reveals that the different sample regions are dominated by one of the components, Fe or Ni, but a slight mixing between the components can be found (see Figure 1), which was confirmed with X-ray Diffraction (XRD). XPS indicates the enrichment of Fe at the sample surface, while HAXPES and EDS data agree on the stoichiometry of the bulk. High-resolution XPS and HAXPES exhibit some differences in the valence states of Fe and Ni, whereas Ni seems to be easier to reduce than Fe. Further investigations combining these different techniques and additionally Secondary Ion Mass Spectrometry (ToF-SIMS) are ongoing by using in situ approaches and coupling cyclic voltammetry to the analytical techniques. T2 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - Oxygen evolution reaction KW - Transmission Electron Microscopy KW - (Hard) X-ray Photoelectron Spectroscopy KW - Synergistic effects PY - 2024 AN - OPUS4-60534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Standardisation needs for regulatory testing of graphene and related 2D materials. phy-chem properties N2 - The main properties and main methods which are needed for the physico-chemical characterisation of graphene related 2D materials are discussed. As expample for standardization, protocols for the measurement of the chemical composition with XPS are discussed. The results of an interlaboratory comparisons led to new recommendations for the reliable measurments protocols. T2 - Materials Week 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Standardisation KW - Functionalized graphene KW - Interlaboratory comparison KW - Endpoints PY - 2024 AN - OPUS4-60537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Interlaboratory comparisons as tool in advanced materials characterisation N2 - Interlaboratory comparisons (ILCs) are an important tool for the validation of characterisation methods, and, herwith, a prerequisite for standardisation. The "Versailles Project on Advanced Materials and Standards" offers a framework for performing such ILCs: (i) TiO2 nanoparticles using ToF-SIMS, and (ii) the chemical composition of functionalized graphene using XPS. The results of both ILCs underline the importance of sample preparation for the measured results. T2 - NanoMeasure France Meeting CY - Online meeting DA - 07.06.2024 KW - Standardisation KW - Validation KW - Interlaboratory comparison KW - Graphene related 2D materials KW - Titania nanoparticles PY - 2024 AN - OPUS4-60532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - da Costa, P. F. G. M. A1 - Merízio, L. G. A1 - Wolff, N. A1 - Terraschke, H. A1 - de Camargo, Andrea Simone Stucchi T1 - Real-time monitoring of CdTe quantum dots growth in aqueous solution N2 - Quantum dots (QDs) are remarkable semiconductor nanoparticles, whose optical properties are strongly size-dependent. Therefore, the real-time monitoring of crystal growth pathway during synthesis gives an excellent opportunity to a smart design of the QDs luminescence. In this work, we present a new approach for monitoring the formation of QDs in aqueous solution up to 90 °C, through in situ luminescence analysis, using CdTe as a model system. This technique allows a detailed examination of the evolution of their light emission. In contrast to in situ absorbance analysis, the in situ luminescence measurements in reflection geometry are particularly advantageous once they are not hindered by the concentration increase of the colloidal suspension. The synthesized particles were additionally characterized using X-ray diffraction analysis, transition electron microscopy, UV-Vis absorption and infrared spectroscopy. The infrared spectra showed that 3-mercaptopropionic acid (MPA)-based thiols are covalently bound on the surface of QDs and microscopy revealed the formation of CdS. Setting a total of 3 h of reaction time, for instance, the QDs synthesized at 70, 80 and 90 °C exhibit emission maxima centered at 550, 600 and 655 nm. The in situ monitoring approach opens doors for a more precise achievement of the desired emission wavelength of QDs. KW - CdTe quantum dots KW - In situ synthesis KW - Real time growth control PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603596 DO - https://doi.org/10.1038/s41598-024-57810-8 VL - 14 IS - 1 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-60359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Fengchan A1 - Oiticica, Pedro Ramon Almeida A1 - Abad-Arredondo, Jaime A1 - Arai, Marylyn Setsuko A1 - Oliveira, Osvaldo N. A1 - Jaque, Daniel A1 - Fernandez Dominguez, Antonio I. A1 - de Camargo, Andrea Simone Stucchi A1 - Haro-González, Patricia T1 - Brownian Motion Governs the Plasmonic Enhancement of Colloidal Upconverting Nanoparticles N2 - Upconverting nanoparticles are essential in modern photonics due to their ability to convert infrared light to visible light. Despite their significance, they exhibit limited brightness, a key drawback that can be addressed by combining them with plasmonic nanoparticles. Plasmon-enhanced upconversion has been widely demonstrated in dry environments, where upconverting nanoparticles are immobilized, but constitutes a challenge in liquid media where Brownian motion competes against immobilization. This study employs optical tweezers for the three-dimensional manipulation of an individual upconverting nanoparticle, enabling the exploration of plasmon-enhanced upconversion luminescence in water. Contrary to expectation, experiments reveal a long-range (micrometer scale) and moderate (20%) enhancement in upconversion luminescence due to the plasmonic resonances of gold nanostructures. Comparison between experiments and numerical simulations evidences the key role of Brownian motion. It is demonstrated how the three-dimensional Brownian fluctuations of the upconverting nanoparticle lead to an “average effect” that explains the magnitude and spatial extension of luminescence enhancement. KW - Upconversion KW - Plasmon enhancement KW - Optical tweezers KW - Brownian motion KW - Nanoparticles PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603551 DO - https://doi.org/10.1021/acs.nanolett.4c00379 VL - 24 IS - 12 SP - 3785 EP - 3792 PB - American Chemical Society (ACS) AN - OPUS4-60355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fernandez-Poulussen, D. A1 - Hodoroaba, Vasile-Dan A1 - Drobne, D. A1 - Novak, S. A1 - Kranjc, E. A1 - Pellegrino, F. A1 - Gullumian, M. A1 - Jones, E. A1 - Hardy, B. A1 - Valsami-Jones, E. A1 - Jurkschat, K. A1 - van der Zande, M. T1 - Holistic, reliable and practical Characterization Framework for Graphene Family Materials, a correlated approach including Imaging based techniques N2 - ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022. T2 - MaterialsWeek 2024 CY - Limassol, Cyprus DA - 17.06.2024 KW - Graphene KW - Graphene-related 2D materials KW - SSbD KW - Imaging KW - ACCORDs PY - 2024 AN - OPUS4-60573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Hörmann, Anja A1 - Moradi, Melika A1 - Smales, Glen Jacob A1 - Breßler, Ingo A1 - Moeez, Abdul T1 - Laboratory x-ray scattering instruments as agile test-beds towards holistic experimentation N2 - Laboratory sources offer a unique advantage compared to synchrotron sources, largely in terms of freedom of operation. This freedom from user obligations, technology and software stacks and legacy decisions make the laboratory a very flexible place to develop and explore new ideas. The unparalleled availability furthermore allows for iterative improvement of instrumentation, sample environments and measurement methodologies to maximise the quality of the data obtained. This talk will highlight the use of the laboratory as an agile test-bed and development space, by giving examples of some complete and incomplete investigations undertaken in our laboratory over the last years. Furthermore, it will introduce the concept of holistic experimentation, where the laboratory provides broad-ranging support for materials science investigations. This means that we assist in the experimental preparation, perform the measurements, correction and analysis, and follow-up with assistance in interpretation of our analyses in light of the results from other techniques applied to the investigation. T2 - Invited talk at Diamond Light Source CY - Didcot, UK DA - 22.05.2024 KW - X-ray scattering KW - Methodology development KW - Laboratory management KW - Holistic experimentation KW - Laboratory automation KW - Nanostructural analysis PY - 2024 AN - OPUS4-60582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Chambers, Aaron P. A. A1 - Hörmann, Anja A1 - Frontzek, Julius A1 - Du, Bofeng A1 - Breßler, Ingo T1 - Getting down to business: pragmatic solutions for laboratory automation N2 - A chemical engineer by training, Brian drifted towards physics and now focuses on a broad spectrum of activities with the aim to improve scientific reproducibility. This includes studies on holistically improving data quality, data collection efficiency and traceability, as well as concomitant laboratory automation for the preparation of consistent, well-documented sample series. The need for pragmatism led to an inexpensive, flexible laboratory automation platform that can be implemented in a modest amount of time. This talk presents that effort. T2 - Future Labs Live 2024 CY - Basel, Switzerland DA - 25.06.2024 KW - Laboratory automation KW - Experiment tracking KW - Holistic experimentation KW - Experimental traceability KW - Data visualisation KW - Parameter correlation. PY - 2024 AN - OPUS4-60583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Structuring of thin films by ultrashort laser pulses N2 - Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications. KW - Thin films KW - Laser processing KW - Ultrashort lasers KW - Laser damage KW - Femtosecond laser ablation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565732 DO - https://doi.org/10.1007/s00339-022-06229-x SN - 0947-8396 SN - 1432-0630 VL - 129 IS - 1 SP - 1 EP - 38 PB - Springer CY - Berlin AN - OPUS4-56573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - The SPONGE v.1.0.0: Modeling scattering of shapes by STL input, with absolute intensities and size distribution. N2 - Simulates X-ray and Neutron scattering patterns from arbitrary shapes defined by STL files. Features: - Uses multithreading to compute a number of independent solutions, then uses the variance of the results to estimate an uncertainty on the output. - Can be launched from the command line using an excel sheet to define settings, or from a jupyter notebook. - Outputs scattering patterns in absolute units if the contrast is set. - A Gaussian size distribution is available, where the relative scaling of objects for each repetion can be varied. Recommended to be used with limited width (max. 10%) to avoid artefacts. - Writes results with settings to an archival HDF5 file. Application examples: This software has been used in several studies to date. For example, it has been used here to simulate a model scattering pattern for a cuboid shape, which was then fed forward into the McSAS3 analysis program for analyzing scattering patterns of polydisperse cuboids. A second use is here, where it was used for the modeling of flattened helices. In this paper, scattering pattern features could be matched with particular morphological changes in the structure. Lastly, this paper has an example where it was used to validate the analytical analysis model, and explore the realistic limits of application of the analytical model. KW - Software KW - Scattering pattern analysis KW - Scattering pattern simulation KW - X-ray KW - Neutron KW - Command-line interface KW - Scattering pattern KW - STL file input KW - Python KW - Arbitrary shapes PY - 2023 DO - https://doi.org/10.6084/m9.figshare.21857130.v1 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-56815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Liu, Y. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Long, W. A1 - Ou, J. T1 - NaYF4:Yb3+/Tm3+@NaYF4:Yb3+ Upconversion Nanoparticles for Optical Temperature Monitoring and Self-Heating in Photothermal Therapy N2 - The core−shell NaYF4:Yb3+/Tm3+@NaYF4:Yb3+ upconversion nanoparticles were successfully prepared by a solvothermal method, and a layer of mesoporous silica (mSiO2) was successfully coated on the periphery of the core−shell nanoparticles to transform their surface from lipophilic to hydrophilic, further expanding their applications in biological tissues. The physical phase, morphology, structure, and fluorescence properties were characterized by X-ray diffraction (XRD), field emission transmission electron microscopy (TEM), Fourier infrared spectroscopy (FT-IR), ζ potential analysis, and fluorescence spectroscopy. It was found that the material has a hexagonal structure with good hydrophilicity and emits intense fluorescence under 980 nm pump laser excitation. The non-contact temperature sensing performance of nanoparticles was evaluated by analyzing the upconversion fluorescence of Tm3+ (1G4 → 3F4 and 3F3 → 3H6) in the temperature range of 284−344 K. The absolute and relative sensitivities were found to be 0.0067 K−1 and 1.08 % K−1, respectively, with high-temperature measurement reliability and good temperature cycling performance. More importantly, its temperature measurement in phosphate-buffered saline (PBS) solution is accurate. In addition, the temperature of the cells can be increased by adjusting the laser power density and laser irradiation time. Therefore, an optical temperature sensing platform was built to realize the application of real-time monitoring of cancer cell temperature and the dual function of photothermal therapy. KW - Sensor KW - Temperature KW - Lanthanide KW - Tag KW - Fluorescence KW - Nanoparticles KW - Synthesis KW - Environment KW - Monitoring KW - Sensing KW - Nano KW - Life sciences KW - Upconversion PY - 2023 DO - https://doi.org/10.1021/acsanm.2c05110 VL - 6 IS - 1 SP - 759 EP - 771 PB - ACS Publications AN - OPUS4-57081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Li, Z. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Long, W. A1 - Ou, Jun T1 - Preparation of NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles and application of their fluorescence temperature sensing properties N2 - The NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles were successfully prepared by the solvothermal method, and the samples were pure hexagonal phase with good crystallinity and homogeneous size, asevidenced by XRD and TEM analysis. The FT-IR analysis shows that β-CD is successfully encapsulated on the surface of NaYF4: Yb3+/Tm3+@NaYF4 nanoparticles. The fluorescence intensity 3and lifetime were significantly increased after coating the inert layer on the surface of core nanoparticles. After further surface modification of β-CD, the fluorescence intensity and fluorescence lifetime were reduced, but the overall fluorescence was stronger. Temperature measurements using the fluorescence intensity ratio technique were found to have relatively low reliability and absolute sensitivity for temperature measurements using thermally coupled energy levels. However, the reliability of temperature measurements using non-thermally coupled energy levels is significantly higher and the absolute sensitivity is much higher than for measurements at thermally coupled levels. Since the maximum absolute sensitivity, maximum relative sensitivity and minimum temperature resolution are determined to be 0.1179 K-1, 2.19 %K􀀀 1 and 0.00019 K, respectively, NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles are expected to be widely used in the biomedical field due to their feasibility, reliability, non-toxicity and harmlessness. KW - Upconversion KW - Surface modification KW - Fluorescence intensity ratio KW - Thermally coupled levels KW - Non-thermally coupled levels PY - 2023 DO - https://doi.org/10.1016/j.optmat.2022.113389 SN - 0925-3467 VL - 136 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-57105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cheng, Z. A1 - Meng, M. A1 - Qiao, X. A1 - Liu, Y. A1 - Resch-Genger, Ute A1 - Ou, J. T1 - The synthesis of Er3+/Yb3+/K+ triple-doped NaYF4 phosphors and its high sensitivity optical thermometers at low power N2 - Optical Thermometry is popular among researchers because of its non-contact, high sensitivity, and fast measurement properties. In the present experiment, Er3+/Yb3+/K+ co-doped NaYF4 nanoparticles with different K+ concentrations were synthesized by solvothermal method, and the samples showed bright upconversion green emission under the excitation of a 980 nm laser. The powder X-ray diffractometer and transmission electron microscope were used to characterize the crystal structure and its surface morphology, respectively. The spectral characteristics of nanoparticles with K+ doping concentration from 10% to 30% (Molar ratio) were investigated by fluorescence spectroscopy, and it was observed that the fluorescence intensity reached the maximum at the K+ concentration of 20%, after which the intensity weakened when the K+ content continued to increase. According to the dependence between the luminescence intensity of the sample and the laser power density and fluorescence lifetime, the intrinsic mechanism was carefully investigated. Temperature-dependent spectra of the samples were recorded in the temperature range of 315–495 K, and the maximum values of absolute sensitivity (Sa) and relative sensitivity (Sr) were measured at 0.0041 K−1 (455 K) and 0.9220%K−1 (315 K). The experimental results show that K+/Er3+/Yb3+ triple-doped NaYF4 green fluorescent nanoparticles (GFNs) have good prospects for applications in display devices, temperature sensing, and other fields. KW - K+ doped KW - Upconversion luminescence KW - Optical temperature sensing KW - Thermal coupling energy level PY - 2023 DO - https://doi.org/10.1016/j.jallcom.2022.168299 VL - 937 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-57106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas A1 - François, P. A1 - Hoffmann, J. A1 - Kaja, K. A1 - Fabricius, N. A1 - Ermilova, Elena A1 - Sachse, René A1 - Gautier, B. T1 - ELENA Project: Creating a simplified uncertainty calculation for industrial applications N2 - In this workpackage of the ELENA project, we develop a way to express the measurement uncertainty of nanoscale determination of electrical propserties. The method developed aims to be usable for industrial contexts and described in technical documents and standards drafts. Standards and reference samples are used to make traceable measurements available for the end user. T2 - Congrès International de Metrologie CY - Lyon, France DA - 06.03.2023 KW - Nanoscale measurements KW - Electrical properties KW - Optical measurements KW - Surfaces KW - Scanning probe measurements PY - 2023 AN - OPUS4-57155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Müller, P. A1 - Babick, F. A1 - Friedrich, C. M. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Mech, A. A1 - Weigel, S. A1 - Wohlleben, W. A1 - Rauscher, H. T1 - NanoDefiner Framework and e-Tool Revisited According to the European Commission’s Nanomaterial Definition 2022/C 229/01 N2 - The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and its e-tool implementation presented here are such instruments, which help stakeholders to find out in a straightforward way whether a material is a nanomaterial or not. They are two major outcomes of the NanoDefine project, which is explicitly referred to in the new definition. This work revisits the framework and e-tool, and elaborates necessary adjustments to make these outcomes applicable for the updated recommendation. A broad set of case studies on representative materials confirms the validity of these adjustments. To further foster the sustainability and applicability of the framework and e-tool, measures for the FAIRification of expert knowledge within the e-tool’s knowledge base are elaborated as well. The updated framework and e-tool are now ready to be used in line with the updated recommendation. The presented approach may serve as an example for reviewing existing guidance and tools developed for the previous definition 2011/696/EU, particularly those adopting NanoDefine project outcomes. KW - Nanomaterial definition KW - Nanomaterial categorisation KW - Nanomaterial regulation KW - Nanomaterial legislation KW - Decision support KW - FAIRification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571618 DO - https://doi.org/10.3390/nano13060990 SN - 2079-4991 VL - 13 IS - 6 - Special Issue "Identification and Quantification of Nanomaterials" SP - 1 EP - 16 PB - MDPI CY - Basel, CH AN - OPUS4-57161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Exkurs Partikelgrößenverteilungen N2 - Einführung in die Darstellung der Ergebnisse von Partikelgrößenbestimmungen: Was ist ein Kugeläquivalenzdurchmesser; welche Bedeutung hat die gemessene Mengenart; welche Parameter werden ausgewiesen. Bezug zu Regularien hinsichtlich der Bewertung "Nano- oder nicht Nano-Material. T2 - BAM Akademie: Info-Tage "NANO OR NOT NANO" CY - Online meeting DA - 16.02.2023 KW - Nano material KW - Particle size KW - Size distribution PY - 2023 AN - OPUS4-57127 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Dynamische Lichtstreuung DLS nach ISO 22412:2017 N2 - Einführung in die Partikelgrößenbestimmung von Nano-Materialien mittels Dynamischer Lichtstreuung. Normative Grundlagen (ISO 22412 und OECD TG 125); Messprinzip, Auswertealgorithmen, Informationsgehalt der Daten, Metadaten, Reporting. T2 - BAM Akademie: Info-Tage "NANO OR NOT NANO" CY - Online meeting DA - 16.02.2023 KW - DLS KW - Particle size KW - Nano PY - 2023 AN - OPUS4-57128 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Zentrifugen Sedimentationsverfahren CLS nach ISO 13318 2:2007 N2 - Einführung in die Bestimmung der Partikelgröße von Nano-Materialien mittels Zentrifugen Sedimentationsverfahren CLS nach ISO 13318 2:2007. Normative Grundlagen (einschließlich OECD TG 125), Messprinzip, Auswertung, Vor- und Nachteile der Methode, Metadaten, Reporting. T2 - BAM Akademie: Info-Tage "NANO OR NOT NANO" CY - Online meeting DA - 16.02.2023 KW - CLS KW - Particle size KW - Nano PY - 2023 AN - OPUS4-57129 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolff, M. A1 - Wonneberger, R. A1 - Freiberg, K.E. A1 - Hertwig, Andreas A1 - Bonse, Jörn A1 - Giebeler, L. A1 - Koitzsch, A. A1 - Kunz, C. A1 - Weber, H. A1 - Hufenbach, J.K. A1 - Müller, F.A. A1 - Gräf, S. T1 - Formation of laser-induced periodic surface structures on Zr-based bulk metallic glasses with different chemical composition N2 - 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. KW - Bulk metallic glasses KW - Femtosecond laser KW - Laser-induced periodic surface structures (LIPSS) KW - Chemical analysis KW - Oxidation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581799 DO - https://doi.org/10.1016/j.surfin.2023.103305 SN - 2468-0230 VL - 42 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-58179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed A. A1 - Juranyi, Fanni A1 - Böhning, Martin A1 - Zorn, Reiner A1 - Schönhals, Andreas T1 - Low-Frequency Vibrational Density of State of Janus-Polynorbornenes: The Dependence of the Boson Peak on the Nanophase-Separated Structure N2 - Inelastic incoherent neutron time-of-flight scattering was employed to investigate the low-frequency vibrational density of states (VDOSs) for a series of glassy Janus-poly(tricyclononenes), which consist of a rigid main chain and flexible alkyl side chains. Here, the length of the flexible side chains was systematically varied from propyl to octyl. Such materials have potential applications as active separation layers in gas separation membranes as a green future technology, especially for the separation of higher hydrocarbons. From the morphological point of view, the Janus polynorbornenes undergo a nanophase separation into alkyl side chain-rich nanodomains surrounded by a rigid polynorbornene matrix. Here, the influence of the nanophase-separated structure on the low-frequency VDOS is investigated from a fundamental point of view. The low-frequency VDOSs of these Janus polynorbornene show excess contributions to the Debye type VDOS known as the Boson peak (BP) for all side chain lengths. Due to the high incoherent scattering cross-section of hydrogen, most of the scattering comes from the alkyl side chain-rich domains. Compared to conventional glass-forming materials, in the considered Janus polynorbornenes, the BP has a much lower intensity and its frequency position is shifted to higher values. These experimental results are discussed in terms of the nanophase-separated structure where the alkyl chain-rich domains were constrained by the surrounding matrix dominated by the rigid backbone. With increasing alkyl chain length, the size of the alkyl chain-rich domains increases. The frequency position of the BP shifts linearly to lower frequencies with the size of these nanodomains estimated from X-ray measurements. The obtained results support the sound wave interpretation to the BP KW - Inelastic neutron scattering PY - 2023 DO - https://doi.org/10.1021/acs.macromol.3c00913 SN - 0024-9297 SP - 1 EP - 10 PB - ACS AN - OPUS4-57972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andresen, Elina A1 - Islam, Fahima A1 - Prinz, Carsten A1 - Gehrmann, P. A1 - Licha, K. A1 - Roik, Janina A1 - Recknagel, Sebastian A1 - Resch-Genger, Ute T1 - Assessing the reproducibility and up‑scaling of the synthesis of Er,Yb‑doped NaYF4‑based upconverting nanoparticles and control of size, morphology, and optical properties N2 - Lanthanide-based, spectrally shifting, and multi-color luminescent upconverting nanoparticles (UCNPs) have received much attention in the last decades because of their applicability as reporter for bioimaging, super-resolution microscopy, and sensing as well as barcoding and anti-counterfeiting tags. A prerequisite for the broad application of UCNPs in areas such as sensing and encoding are simple, robust, and easily upscalable synthesis protocols that yield large quantities of UCNPs with sizes of 20 nm or more with precisely controlled and tunable physicochemical properties from lowcost reagents with a high reproducibility. In this context, we studied the reproducibility, robustness, and upscalability of the synthesis of β-NaYF4:Yb, Er UCNPs via thermal decomposition. Reaction parameters included solvent, precursor chemical compositions, ratio, and concentration. The resulting UCNPs were then examined regarding their application-relevant physicochemical properties such as size, size distribution, morphology, crystal phase, chemical composition, and photoluminescence. Based on these screening studies, we propose a small volume and high-concentration synthesis approach that can provide UCNPs with different, yet controlled size, an excellent phase purity and tunable morphology in batch sizes of up to at least 5 g which are well suited for the fabrication of sensors, printable barcodes or authentication and recycling tags. KW - Photoluminescence KW - Nano KW - Nanomaterial KW - Synthesis KW - Reproducibility KW - Upconversion nanoparticle KW - Lanthanide PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570170 DO - https://doi.org/10.1038/s41598-023-28875-8 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 13 AN - OPUS4-57017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwibbert, Karin A1 - Richter, Anja M. A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Laser-Textured Surfaces: A Way to Control Biofilm Formation? N2 - Bacterial biofilms pose serious problems in medical and industrial settings. One of the major societal challenges lies in the increasing resistance of bacteria against biocides used in antimicrobial treatments, e.g., via overabundant use in medicine, industry, and agriculture or cleaning and disinfection in private households. Hence, new efficient bacteria-repellent strategies avoiding the use of biocides are strongly desired. One promising route to achieve bacteria-repellent surfaces lies in the contactless and aseptic large-area laser-processing of technical surfaces. Tailored surface textures, enabled by different laser-processing strategies that result in topographic scales ranging from nanometers to micrometers may provide a solution to this challenge. This article presents a current state-of-the-art review of laser-surface subtractive texturing approaches for controlling the biofilm formation for different bacterial strains and in different environments. Based on specific properties of bacteria and laser-processed surfaces, the challenges of anti-microbial surface designs are discussed, and future directions will be outlined. KW - Antibacterial surfaces KW - Biofilms KW - Laser processing KW - Laser-induced periodic surface structures (LIPSS) KW - Microbial adhesions PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588260 DO - https://doi.org/10.1002/lpor.202300753 SN - 1863-8899 SP - 1 EP - 41 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-58826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Srivastava, Priyanka A1 - Tavernaro, Isabella A1 - Scholtz, Lena A1 - Genger, C. A1 - Welker, P. A1 - Schreiber, Frank A1 - Meyer, Klas A1 - Resch-Genger, Ute T1 - Dual color pH probes made from silica and polystyrene nanoparticles and their performance in cell studies N2 - Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability. KW - Sensors KW - Silica and polystyrene nanoparticles KW - pH probe KW - Fluorescence spectroscopy KW - Cell studies KW - Dye KW - Particle synthesis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569198 DO - https://doi.org/10.1038/s41598-023-28203-0 SN - 2045-2322 VL - 13 IS - 1 SP - 1321 EP - 1336 PB - Nature CY - London AN - OPUS4-56919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas A1 - Ermilova, Elena T1 - Ellipsometry as a production measurement tool N2 - Spectroscopic Ellipsometry is an enormously versatile measurement tool for surfaces and thin layers. We discuss the use of ellipsometry in the context of quality control in production processes of eletrconic devices. T2 - Photonics Days Berlin Brandenburg CY - Berlin, Germany DA - 09.10.2023 KW - Ellipsometry KW - Quality control KW - Metrology PY - 2023 AN - OPUS4-59837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena A1 - Weise, Matthias A1 - Hertwig, Andreas T1 - Multi-scale optical imaging methods for quality control of electronic devices N2 - The presentation demonstrates an application of multi-scale optical imaging methods such as spectroscopic imaging ellipsometry and white light interference microscopy for the investigation of wide-bandgap semiconductors for power electronics. The capabilities of these methods for the development of new reference calibration samples for scanning microwave microscopes (SMM) and conductive atomic force microscopes (C AFM) are discussed. T2 - Photonics Days Berlin Brandenburg 2023 CY - Berlin, Germany DA - 09.10.2023 KW - Imaging ellipsometry KW - White light interference microscopy KW - Power electronics KW - Reference standards KW - Metrology KW - Nanoelectronics PY - 2023 AN - OPUS4-59838 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thünemann, Andreas T1 - SAXS for the development of reference materials: Silver nanoparticles, a case study N2 - Today there are hundreds of products available containing silver in form of nanoparticles, so-called nanosilver. This situation and the foreseeable future growing market of nanosilver will supposedly cause an increased release of silver into the environment. In this way, silver can be also incorporated into the human body and accumulated in different organs, which can be toxic or at least an unknown risk to human health. For these reasons, it is important to constantly study materials containing silver nanoparticles, their production, application in products and technical processes, dissemination of silver nanoparticles in the environment, and effects on humans and nature. The state-of-the-art nanoparticle size and concentration characterization are illustrated in an extensive interlaboratory comparison. To guarantee the traceability of measurements and to secure the comparison of results of different analytical methods, reference materials (RM) and certified reference materials (CRM) are essential. As a case study, the objective of the presented project was to provide an aqueous suspension of silver nanoparticles as a reference material with a nominal diameter below 10 nm for application in the determination of the size and concentration of nanoparticles in an aqueous surrounding. Measurands are the particles’ diameter D, size distribution width σ, number density N, and concentration c. Target uncertainties, defined as one sigma of the measurand values, are 5% for D, 10% for σ, 20% for N, and 20% for c. The certification was carried out based on ISO 17867 and the relevant ISO-Guides to produce reference material. The process of using SAXS as a reliable method for testing homogeneity and short-term and long-term stability of the material is reported. The particle preparation is described in detail so that the user can carry out the steps of synthesis and characterization in his own laboratory if required. Optionally, one can also contact the author for the provision of the silver nanoparticles. Detailed information can be found elsewhere (BAM Certification Reports, BAM-N008 (2022)). T2 - SAXS excites CY - Graz, Austria DA - 04.04.2023 KW - Nanoparticles KW - SAXS KW - Nanosilver KW - Small-angle x-ray scattering PY - 2023 AN - OPUS4-57283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoell, A. A1 - Heimann, M. A1 - Wegner, Karl David A1 - Haas, S. A1 - Emmerling, Franziska A1 - Schorr, S. T1 - On the usage of anomalous SAXS to analyzethe structure and composition of bimetallic nanoparticles and quantum dots N2 - Tailor-made nanoparticles are of increasing interest in e.g. catalysis, as sensor materials, analytical assays, or can have superior photophysical properties. A major issue concerning the preparation of high-quality and functional nanoparticles is a good control of particle size, shape, polydispersity, and composition. Small Angle X-ray Scattering (SAXS) is a non-destructive method for the analysis of nanostructures in a wide variety of materials. This method allows determining averaged structural parameters on a length scale from just above atomic sizes up to several 100 nanometers such as sizes, size distributions, volume fractions, and inner surface sizes. Moreover, anomalous Small Angle X-ray Scattering (ASAXS) exploits the anomalous dispersion of the scattering amplitudes near the X-ray absorption edges of the elements contained in the sample. These element sensitive contrast variations can be used to analyse average composition fluctuations on the nm scale. Two kinds of nanoparticles are chosen here to elaborate the advantages of ASAXS in the analysis of complex materials. A facile and efficient methodology is developed for the thermal synthesis of size-tunable, stable, and uniform bimetallic NiCu core–shell nanoparticles (NPs) for various application in catalysis. Their diameter can be tuned in a range from 6 nm to 30 nm and the Ni:Cu ratio is adjustable in a wide range from 1:1 to 30:1. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering (ASAXS), X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Here, we focus on the ASAXS method and its ability to analyses nanostructure parts and their compositions at once. As a result, a NiCu alloyed core surrounded by a Ni enriched shell and an outer NiO shell was found. Semiconductor nanocrystals (quantum dots, QDs) are well known for their superior photophysical properties and enabled advancements in several key technologies of the 21st century and numerous technological applications like in photovoltaics, LED displays, photocatalysis, and biosensing. To achieve high photoluminescence quantum yields (PLQY) and enhanced photostability the QD core needs to be passivated by a second semiconductor, which possess a larger band gap to confine the charges within the QD core. An important parameter is thereby the lattice mismatch between the core and shell. To avoid strong lattice strain, which would alter the photophysical properties, an intermediary shell can be used as a lattice adapter between the core and the outer shell leading to core/shell/shell systems. These systems have shown to possess high PLQYs combined with a strong long-term stability and can be found in modern QLED displays. ASAXS was used here to better understand the core/shell/shell structure of InP/ZnSe/ZnS QDs to enable a correlation between their structural and photophysical properties. T2 - IUCr - International Union of Crystallography CY - Melbourne, Australia DA - 22.08.2023 KW - ASAXS KW - Quantum dot KW - Core/shell materials KW - Safer by design PY - 2023 AN - OPUS4-58812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David A1 - Coro, A. A1 - Marquez, R. M. A1 - Le Guevel, X. A1 - Juarez, B. H. A1 - Resch-Genger, Ute T1 - Exploring the photoluminescence of gold NCs and Ag2S NPs to boost their SWIR emission N2 - Current challenges and objectives for non-invasive optical bioimaging are deep tissue penetration, high detection sensitivity, high spatial and temporal resolution, and fast data acquisition. A promising spectral window to tackle these challenges is the short-wave infrared (SWIR) ranging from 900 nm to 1700 nm where scattering, absorption, and autofluorescence of biological components are strongly reduced compared to the visible/NIR. At present, the best performing SWIR contrast agents are based on nanomaterials containing toxic heavy-metal ions like cadmium or lead, which raises great concerns for biological applications. Promising heavy-metal free nanoscale candidates are gold nanoclusters (AuNCs) and Ag2S nanoparticles (NPs). The photoluminescence (PL) of both types of nanomaterials is very sensitive to their size, composition of their surface ligand shell, and element composition, which provides an elegant handle to fine-tune their absorption and emission features and boost thereby the size of the signals recorded in bioimaging studies. Aiming for the development of SWIR contrast agents with optimum performance, we dived deeper into the photophysical processes occurring in these nanomaterials, thereby exploring in depth how the environment, surface ligand composition, and the incorporation of transition metals influence the optical properties of AuNCs and Ag2S NPs. We observed a strong enhancement of the SWIR emission of AuNCs upon exposure to different local environments (in solution, polymer, and in the solid state). Addition of metal ions such as Zn2+ to Ag2S based NPs led to a strong PL enhancement, yielding PL quantum yields of about 10% and thus making them highly suitable for non-invasive deep imaging of vascular networks and 3D fluid flow mapping. T2 - NaNaX 10 - Nanoscience with Nanocrystals CY - Klosterneuburg, Austria DA - 03.07.2023 KW - Quantum dots KW - Ag2S KW - Fluorescence KW - SWIR KW - Gold nanocluster KW - Nanomaterial KW - bioimaging PY - 2023 AN - OPUS4-58104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Pauli, J. A1 - Güttler, Arne A1 - Richter, Maria A1 - Fiedler, Saskia A1 - Frenzel, Florian A1 - Wegner, Karl David A1 - Würth, Christian T1 - Photoluminescence Quantum Yields of Luminescent Nanocrystals and Particles in the UV/vis/NIR/SWIR N2 - The rational design of functional luminescent materials such as semiconductor quantum dots and lanthanide-based upconversion nanoparticles, all photophysical and mechanistic studies, and the comparison of different emitters require accurate and quantitative photoluminescence measurements. Particularly the reliable determination of the key performance parameter photoluminescence quantum yield (f), the number of emitted per absorbed photons, and the brightness are of special importance for luminescence applications in the life and material sciences and nano(bio)photonics.[1] In this context, examples for absolute measurements of the photoluminescence quantum yields of UV/vis/NIR/SWIR emissive semiconductor quantum dots and rods, made from different materials, and spectrally shifting lanthanide upconversion nanocrystals with different surface chemistries in transparent matrices are presented including excitation wavelength and power density dependent studies utilizing integration sphere spectroscopy.[2,3] In addition, procedures for the absolute determination of the photoluminescence quantum yields of scattering dispersions of larger size quantum rods and differently sized inorganic particles have been developed as well as procedures for the characterization of solid luminescent nanomaterials such as different perovskites and YAG:Cer converter materials.[4] Thereby, challenges and pitfalls of f measurements in different wavelength regions including the SWIR and material-specific effects related to certain emitter classes are addressed, achievable uncertainties are quantified, and relative and absolute measurements of photoluminescence quantum yield measurements are compared to underline limitations of the former approach. Finally, a set of novel UV/vis/NIR quantum yield standards is presented including their certification with a complete uncertainty budget.[5] T2 - NANAX 10 CY - Klosterneuburg, Austria DA - 03.07.2023 KW - Fluorescence KW - Optical spectroscopy KW - Reference data KW - Traceability KW - NIR KW - Scattering KW - Reference material KW - Certification KW - Quality assurance KW - Dye KW - Reference product KW - SWIR KW - Nano KW - Particle KW - Perovskite KW - Integrating sphere spectroscopy KW - Quantum yield PY - 2023 AN - OPUS4-58238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrandt, Jana A1 - Thünemann, Andreas T1 - Aqueous Dispersions of Polypropylene: Toward Reference Materials for Characterizing Nanoplastics N2 - Microplastics and nanoplastics pollute the natural environment all over the world, but the full extent of the hazards posed by this waste is unclear. While research on microplastics is well advanced, little work has been done on nanoplastics. This discrepancy is mainly due to the lacking ability to detect nanoplastics in biologically and environmentally relevant matrices. Nanoplastics reference materials can help the development of suitable methods for identifying and quantifying nanoplastics in nature. The aim is to synthesize nanoplastics made from one of the most commonly used plastics, namely polypropylene. An easy way to produce long-term stable aqueous dispersions of polypropylene nanoparticles (nano polypropylene) is reported. The nanoplastic particles, prepared by mechanical breakdown, show a mean hydrodynamic diameter of D h = 180.5 ± 5.8 nm and a polydispersity index of PDI = 0.084 ± 0.02. No surfactant is needed to obtain dispersion which is stable for more than 6 months. The colloidal stability of the surfactant-free nano polypropylene dispersions is explained by their low zeta potential of 𝜻 = −43 ± 2 mV. KW - Nanoparticles KW - Reference Material KW - Nanoplastics PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571799 DO - https://doi.org/10.1002/marc.202200874 SN - 1022-1336 VL - 44 IS - 6 SP - 1 EP - 15 PB - Wiley-VCH CY - Weinheim AN - OPUS4-57179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pérez Blanes, H. A1 - Ghiasi, Pouria A1 - Sandkühler, J. A1 - Yesilcicek, Yasemin A1 - Pentzien, Simone A1 - Conradi, Andrea A1 - Prinz, Carsten A1 - Al-Sabbagh, Dominik A1 - Thünemann, Andreas A1 - Özcan Sandikcioglu, Özlem A1 - Witt, Julia T1 - High CO2 reduction activity on AlCrCoCuFeNi multi-principal element alloy nanoparticle electrocatalysts prepared by means of pulsed laser ablation N2 - Noble metal-free nanoparticles (NPs) based on multi-principal element alloys (MPEAs) were synthesized using a one-step pulsed laser ablation in liquids (PLALs) method for the electrochemical reduction of CO2. Laser ablation was performed in pure water or poly-(diallyldimethylammonium chloride) (PDADMAC)-containing an aqueous solution of Al8Cr17Co17Cu8Fe17Ni33 MPEA targets. Transmission electron microscopy (TEM) measurements combined with energy dispersive X-ray (EDX) mapping were used to characterize the structure and composition of the laser-generated MPEA nanoparticles (MPEA-NPs). These results confirmed the presence of a characteristic elemental distribution of a core-shell phase structure as the predominant NP species. The electrocatalytic performance of the laser-generated MPEA-NPs was characterized by linear sweep voltammetry (LSV) demonstrating an enhanced electrocatalytic CO2 activity for PDADMAC-stabilized NPs. The findings of these investigations indicate that MPEAs have great potential to replace conventional, expensive noble metal electrocatalysts. KW - Metals and Alloys KW - Surfaces KW - Biomaterials KW - Ceramics and Composites KW - Coatings and Films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588218 DO - https://doi.org/10.1016/j.jmrt.2023.05.143 SN - 2238-7854 VL - 24 SP - 9434 EP - 9440 PB - Elsevier B.V. AN - OPUS4-58821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrandt, Jana A1 - Taubert, Andreas A1 - Thünemann, Andreas T1 - Synthesis and Characterization of Ultra‐Small Gold Nanoparticles in the Ionic Liquid 1‐Ethyl‐3‐methylimidazolium Dicyanamide, [Emim][DCA] N2 - AbstractWe report on gold clusters with around 62 gold atoms and a diameter of 1.15±0.10 nm. Dispersions of the clusters are long‐term stable for two years at ambient conditions. The synthesis was performed by mixing tetrachloroauric acid (HAuCl4 ⋅ 3 H2O) with the ionic liquid 1‐ethyl‐3‐methylimidazolium dicyanamide ([Emim][DCA]) at temperatures of 20 to 80 °C. Characterization was performed with small‐angle X‐ray scattering (SAXS), UV‐Vis spectroscopy, and MALDI‐TOF mass spectrometry. A three‐stage model is proposed for the formation of the clusters, in which cluster growth from gold nuclei takes place according to the Lifshitz‐Slyozov‐Wagner (LSW) model followed by oriented attachment to form colloidal stable clusters. KW - Reference materials KW - SAXS KW - Gold KW - Nanoparticle KW - Small-angle X-ray scattering KW - Ionic liquid PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588203 DO - https://doi.org/10.1002/open.202300106 SN - 2191-1363 VL - 44 SP - 1 EP - 19 PB - Wiley AN - OPUS4-58820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohammad, W. A1 - Wegner, Karl David A1 - Comby-Zerbino, C. A1 - Trouillet, V. A1 - Ogayer, M. P. A1 - Coll, J.-L. A1 - Marin, R. A1 - Jaque Garcia, D. A1 - Resch-Genger, Ute A1 - Antoine, R. A1 - Le Guevel, X. T1 - Enhanced brightness of ultra-small gold nanoparticles in the second biological window through thiol ligand shell control N2 - Gold-based nanoparticles below 2 nm in size are promising as luminescent probes for in vivo bioimaging, owing to their brightness and rapid renal clearance. However, their use as contrast agents in the near-infrared II (NIR-II, 1000–1700 nm) range remains challenging due to their low photoluminescence (PL) quantum yield. To address this, PL enhancement can be achieved by either rigidifying the ligand-shell structure or increasing the size of the ligand shell. In this study, we synthesized ultra-small gold nanoparticles stabilized by co-ligands, namely monothiol and short dithiol molecules. By precisely controlling the amount of reducing agent used during particle preparation, we successfully modulated the physicochemical properties of the co-ligand shell, including its size, composition, and structure. Consequently, we achieved a remarkable 60-fold increase in the absorption cross-section at 990 nm while maintaining the small size of the 1.5-nm metal core. The analytical and optical characterization of our thiol-capped gold nanoparticles indicates that the ligand shell size is governed by the quantity of the reducing agent, which, in turn, impacts the balance between radiative and non-radiative processes, thereby influencing the PL quantum yield. KW - Gold nanocluster KW - NIR-II fluorescence KW - SWIR KW - Nanomaterial design KW - Calibrated fluorescence measurements PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588117 DO - https://doi.org/10.1039/D3TC03021K SN - 2050-7526 VL - 11 IS - 42 SP - 14714 EP - 14724 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kuchenbecker, Petra A1 - Lindemann, Franziska T1 - SOP and reference data for determination of the Volume-specific Surface Area (VSSA) of a commercially available CeO2 nano powder N2 - Detailed SOP and reference data for the determination of the VSSA of a commercially available CeO2 nano powder: specific (BET-) Surface Area by gas adsorption (Ar and N2) skeletal (true solid state) density by gas pycnometry. Estimation of the particle size by VSSA screening method. KW - Nano powder KW - VSSA KW - Volume specific surface area KW - Screening method KW - Ceria KW - CeO2 PY - 2023 DO - https://doi.org/10.5281/zenodo.10061235 PB - Zenodo CY - Geneva AN - OPUS4-58786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shanmugam, Sankaran A1 - Peterlechner, Martin A1 - Iskandar, Mohamad Riza A1 - Saikia, Ujjal A1 - Kulitckii, Vladislav A1 - Lipińska-Chwałek, Marta A1 - Mayer, Joachim A1 - Rösner, Harald A1 - Hickel, Tilmann A1 - Divinski, Sergiy V. A1 - Wilde, Gerhard T1 - Coherent twin-oriented Al3Sc-based precipitates in Al matrix N2 - Al3(Sc,Zr,Ti) nanoparticles with an ideal twin-type orientation relationship to Al host matrix were found in cold-rolled and subsequently annealed Al-based alloy. Atomic-scale investigations using high-resolution scanning transmission electron microscopy identified particles that form prominent coherent (111) twin-type interfaces along their longer facets and semi-coherent twin interfaces on their shorter facets. Ab-initio calculations showed that a coherent Al/Al3Sc twin-like phase boundary corresponds to a local energy minimum. A model is proposed explaining the formation of the twin orientation relationship of an Al3Sc nanoparticle with the Al host matrix. KW - Al-based alloy KW - Precipitation KW - Twin orientation relationship KW - Ab initio calculations KW - Transition electron microscopy PY - 2023 DO - https://doi.org/10.1016/j.scriptamat.2023.115351 SN - 1359-6462 VL - 229 SP - 1 EP - 6 PB - Elsevier BV AN - OPUS4-58789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Rühle, Bastian A1 - Bresch, Harald T1 - Competence Center nano@BAM Welcomes ISO/TC 229 Meeting in Berlin N2 - The Competence Center nano@BAM is presented. Examples directly related to the activities of the ISO Technical Committee TC 229 Nanotechnologies as well as BAM projects on nano reference measurement procedures, nano reference materials and nano reference data sets are showed. T2 - The 32nd ISO/TC 229 IEC/TC 113 JWG2 General Meeting CY - Berlin, Germany DA - 06.11.2023 KW - ISO/TC 229 Nanotechnologies KW - Nanoparticles KW - Nano@BAM KW - Reference materials KW - Reference data KW - Reference procedures PY - 2023 AN - OPUS4-58814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - López-Puertollano, Daniel A1 - Tobias, Charlie A1 - Bell, Jeremy A1 - Abad-Somovilla, A. A1 - Abad Fuentes, A. A1 - Rurack, Knut T1 - Superparamagnetic core-shell particles application: from cytometry assay to simplified fluidic system N2 - Superparamagnetic hybrid polystyrene-core silica-shell beads have emerged as promising alternatives to traditional in flow cytometry-based competitive antibody assays [1]. These materials consist of a polystyrene core and a silica shell, in which magnetic nanoparticles are embedded, facilitating the handling and retention in tests. The outer silica surface allows for easy modification through silane chemistry, allowing the attachment of antibodies, or other molecules of interest. Ochratoxin A (OTA), a mycotoxin that can be found in grain products, coffee, cacao, or grapes, was chosen as the main target analyte to detect [2]. In this study, previously in house produced anti-OTA antibodies [3] were attached to the surface of the particles and the whole system was used as detection entity. In a first approach, the system was used for the development of a competitive cytometry assay using an OTA-fluorescein (OTA-F) adduct as competitor and marker. In this assay the fluorescence emitted by the OTA-F competitor on the surface of the particle was detected at a wavelength of 518 nm using a 533/30.H filter and was correlated to the forward scatter (FSC) to distinguish it from the excess of competitor still in solution. Under optimised conditions, the final assay showed a limit of detection of 0.03 nM. In a second approach, a simplified ready-to-inject fluidic system was built based on a laser (488 nm) and a photomultiplier detector to measure the signal of competitor still in solution. The competition step was carried out in a vial and the whole mixture was injected into the fluidic system. To avoid signal scattering, the particles were separated in-line using a magnet and only the OTA-F competitor still in solution was detected, reaching a limit of detection of 1.2 nM. With the aim to reduce user manipulation, the final assay is still under development for in-line incubation during the competitive step. T2 - 15th Rapid Methods Europe Conference CY - Amsterdam, Netherlands DA - 06.11.2023 KW - Microfluidics KW - Flow cytometry KW - Bead-based assays KW - Magnetic beads KW - Core-shell particles KW - Immunoassays PY - 2023 AN - OPUS4-58817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Andresen, Elina A1 - Würth, Christian A1 - Weigert, Florian A1 - Frenzel, Florian T1 - Functional Luminophores – From Photophysics to Standardized Luminescence Measurements N2 - Inorganic nanocrystals with linear and nonlinear luminescence in the ultraviolet, visible, near infrared and short-wave infrared like semiconductor quantum dots and spectrally shifting lanthanide-based nanophosphors have meanwhile found applications in the life and material sciences ranging from optical reporters for bioimaging and sensing over security barcodes to solid state lighting and photovoltaics. These nanomaterials commonly have increasingly sophisticated core/shell particle architectures with shells of different chemical composition and thickness to minimize radiationless deactivation at the particle surface that is usually the main energy loss mechanism [1]. For lanthanide-based spectral shifters, particularly for very small nanoparticles, also surface coatings are needed which protect near-surface lanthanide ions from luminescence quenching by high energy vibrators like O-H groups and prevent the disintegration of these nanoparticles under high dilution conditions. [2,3,4]. The identification of optimum particle structures requires quantitative spectroscopic studies focusing on the key performance parameter photoluminescence quantum yield [5,6], ideally flanked by single particle studies to assess spectroscopic inhomogeneities on a particle-to-particle level for typical preparation methods [7,8], Moreover, in the case of upconversion nanoparticles with a multi-photonic and hence, excitation power density (P)-dependent luminescence, quantitative luminescence studies over a broad P range are required to identify particle architectures that are best suited for applications in fluorescence assays up to fluorescence microscopy. Here, we present methods to quantify the photoluminescence of these different types of emitters in the vis/NIR/SWIR and as function of P and demonstrate the importance of such measurements for a profound mechanistic understanding of the nonradiative deactivation pathways in semiconductor and upconversion nanocrystals of different size and particle architecture in different environments. T2 - Eingeladener Vortrag Uni Erlangen CY - Erlangen, Germany DA - 18.01.2023 KW - Semiconductor quantum dot KW - Upconversion nanocrystal KW - Luminescence KW - Quantitative spectroscopy KW - Photophysics KW - Quality assurance KW - Nano KW - Particle KW - Quantum yield KW - Lifetime KW - Standard KW - Reference material KW - Surface analysis KW - Quantification PY - 2023 AN - OPUS4-57011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - X-ray Scattering USAXS/SAXS/WAXS (/XRD/PDF) N2 - A ten minute introduction to the technique of X-ray scattering. This talk discusses the foundation and the resulting morphological parameters that can be obtained from the technique. The talk is prepared for discussion within the framework of the OECD REACH guideline for nanomaterials. T2 - Digitaler Info-Tag "Nano or not Nano" CY - Berlin, Germany DA - 16.02.2023 KW - X-ray scattering KW - BAM Academy KW - SAXS KW - XRD KW - WAXS KW - Nanomaterial KW - REACH KW - OECD KW - Guideline PY - 2023 AN - OPUS4-57013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Tavernaro, Isabella A1 - Nirmalananthan-Budau, Nithiya T1 - New project on the quantification of functional groups (FGS) on nanomaterials N2 - The surface chemistry of nanomaterials controls their interaction with the environment and biological species and their fate and is hence also relevant for their potential toxicity. This has meanwhile led to an increasing interest in validated and preferably standardized methods for the determination and quantification of surface functionalities on nanomaterials and initiated different standardization projects within ISO/TC 229 and IEC/TC 113 as well as interlaboratory comparisons (ILCs) of different analytical methods for the quantification of surface coatings by OECD. Here we present the results of a first ILC on the quantification of the amount of amino functionalities on differently sized inorganic nanoparticles done by division Biophotonics and the National Research Council of Canada (NRC) and the PWI 19257 on the Characterization and Quantification of Surface Functional Groups and Coatings on Nanoobjects approved by ISO/TC 229 (WG2) in fall 2022 that will result in a VAMAS study on this topic organized by division Biophotonics. Key words: nanoparticles, surface analysis, surface functional groups, quantification, optical assay, qNMR, VAMAS, standardization, ICL, quality assurance, reference material. T2 - Eingeladener Vortrag Universität Erlangen CY - Erlangen, Germany DA - 18.01.2023 KW - Quality assurance KW - Nano KW - Particle KW - Standard KW - Reference material KW - Surface analysis KW - Quantification KW - Interlaboratory comparison KW - Standardization KW - VAMAS PY - 2023 AN - OPUS4-57044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawek, Marcel A1 - Omar, Hassan A1 - Szymoniak, Paulina A1 - Schönhals, Andreas T1 - Growth kinetics of the adsorbed layer of poly(2-vinylpyridine) - An indirect observation of desorption of polymers from substrates N2 - The growth kinetics of the adsorbed layer of poly(2-vinylpiridine) on silicon oxide is studied using a leaching technique which is based on the Guiselin brushes approach. The adsorbed layer is grown from a 200 nm thick P2VP film for several annealing time periods at different annealing temperatures. Then the film is solvent-leached, and the height of the remaining adsorbed layer is measured by atomic force microscopy. At the lowest annealing temperature only a linear growth regime is observed, followed by a plateau. Here, the molecular mobility of segments is too low to allow for a logarithmic growth. At higher annealing temperatures, both linear and logarithmic growth regimes are observed, followed by a plateau. At even higher annealing temperatures, the growth kinetics of the adsorbed layer changes. A linear growth followed by logarithmic growth kinetics is observed for short annealing time periods. For longer annealing time periods, an upturn of the growth kinetics is observed. At the highest annealing temperature, only a logarithmic growth regime is found. The change in the growth kinetics is discussed by an alteration in the structure of the adsorbed layer. Moreover, the interaction between the polymer segments and the substrate becomes weaker due to both enthalpic and entropic effects. Therefore, at high annealing temperatures the polymer segments might more easily desorb from the substrate. KW - Ultra thin polymer films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575423 DO - https://doi.org/10.1039/d3sm00129f SN - 1744-683X SN - 1744-6848 VL - 19 IS - 21 SP - 3975 EP - 3982 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-57542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -