TY - GEN A1 - Vladár, A. E. A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanoparticles by scanning electron microscopy N2 - In this chapter sample preparation, image acquisition, and nanoparticle size and shape characterization methods using the scanning electron microscope (SEM) in reflective and transmitted working modes are described. These help in obtaining reliable, highly repeatable results. The best solutions vary case-by-case and depend on the raw (powdered or suspension) nanoparticle material, the required measurement uncertainty and on the performance of the SEM. KW - Nanoparticles KW - Sample preparation KW - Electron microscopy KW - SEM KW - Size measurement KW - Shape KW - Threshold PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00002-X SP - 7 EP - 27 PB - Elsevier CY - Amsterdam AN - OPUS4-50120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Ye, M.-Y. A1 - Yang, Q. A1 - Kreyenschulte, C. A1 - Wagner, Andreas A1 - Frisch, M. A1 - Brückner, A. A1 - Kondratenko, E. A1 - Kraehnert, R. T1 - Dynamics of Reaction-Induced Changes of Model-Type Iron Oxide Phases in the CO2-Fischer-Tropsch-Synthesis N2 - Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase. Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed. KW - Nanostructured FeOx films KW - CO2 KW - Scanning Auger Spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549709 DO - https://doi.org/10.1002/cctc.202200240 SN - 1867-3880 VL - 14 IS - 14 SP - 1 EP - 11 PB - Wiley-VCH AN - OPUS4-54970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Wohlleben, W. A1 - Marvin, H. A1 - Weigel, S. A1 - Brüngel, R. A1 - Friedrich, C. M. T1 - The NanoDefine Methods Manual - Part 1: The NanoDefiner Framework and Tools N2 - The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial', funded by the European Union's 7th Framework Programme, under grant agreement 604347. In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms), - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 1. KW - Nanomaterial KW - Nanoparticles KW - NanoDefine KW - Nanoparticle size distribution KW - Nanomaterial classification KW - Framework KW - Tools PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503699 SN - 978-92-76-11950-0 DO - https://doi.org/10.2760/55181 SN - 1831-9424 SP - 1 EP - 89 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Rühle, Bastian A1 - Hodoroaba, Vasile-Dan T1 - Understanding Correlative Electron Microscopy Imaging with SEM, STEM-in-SEM and TEM for the Accurate Characterization of Size and Shape of Iron Oxide Nanoparticles N2 - The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM). For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary. The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM. With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically). ❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility. ❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs. ❑ Selection of the threshold algorithm can significantly alter the reported ECD. KW - Nanoparticles KW - Iron oxide KW - Electron microscopy KW - Reference materials KW - Particle size distribution KW - Imaging PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.339 VL - 30 IS - Supplement_1 SP - 710 EP - 711 PB - Oxford University Press (OUP) AN - OPUS4-61007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Advanced Characterization of the Surface Morphology and Chemistry within nano@BAM N2 - Both essential aspects of the surface of solid matter, its morphology and chemistry, are studied traditionally at BAM starting in the 60’s with different cyclical research focus areas, mostly related either to applicative research or method development. In the recent years, the focus has shifted almost exclusively to the nano-analytics of advanced materials such as complex nanoparticles, (ultra)thin films/coatings, nanocomposites, 2D materials, energy materials, etc. This is also the reason why BAM has established recently the new Competence Center nano@BAM (www.bam.de/Navigation/DE/Themen/Material/Nanotechnologie/sichere-nanomaterialien.html) with the five sub-fields nanoCharacterisation, nanoMaterial, nanoSafety, nanoData and nanoTechnology. The link to the BAM central guidelines to the safety in technology and chemistry is given by the development of reference products such as reference measurement procedures, reference (nano)materials, and newly reference data sets. Thus, an internationally well-networked group in surface analysis has been established @BAM, with regular contributions to integral analytical characterization with metrological and standardization background. Examples of newly developed methodical approaches will be given with an emphasis on correlative nano-analysis of morphology and chemistry of nanomaterials. Correlative imaging by STEM-in-SEM with high-resolution SEM and EDX, and further with AFM or the new technique TKD (Transmission Kikuchi Diffraction) will be explained on various examples of nanostructures, both as starting materials and embedded/functionalized nanoparticles in products. The unique analytical benefits of the Auger electron probe as a veritable nano-tool for surface chemistry will be highlighted. The panoply of advanced surface characterization methods @BAM is completed by discussing examples of hybrid analysis of the bulk of nanomaterials by X-ray Spectroscopy with the highest surface-sensitive methods X-ray Photoelectron Spectroscopy (XPS) and Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). Particularly for the analysis of the surface chemistry of nanostructures, such as the completeness of the shells of core-shell nanoparticles or in-depth and lateral gradients of chemistry within mesoporous thin layers, the latter methods are inherent. Other special developments like approaches for the quantitative determination of the roughness of particle surface by electron microscopy or for the quantitative determination of the porosity of thin mesoporous layers by electron probe microanalysis (EPMA) with SEM will be presented. T2 - Seminar of the Academic Centre for Materials and Nanotechnology CY - Online meeting DA - 12.05.2022 KW - Nanoparticles KW - Thin films KW - Nano Characterisation KW - Nanomaterials KW - Surface morphology KW - Surface chemistry PY - 2022 UR - https://www.agh.edu.pl/en/info/article/seminar-advanced-characterization-of-the-surface-morphology-and-chemistry-within-nanobam/ AN - OPUS4-54820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Hodoroaba, Vasile-Dan T1 - Wire-Print as a Novel Sample Preparation Approach for Accurate Morphological Characterization of Constituent Particles of Graphene-Related 2D-Materials N2 - Graphene and graphene-oxide (GO) are used for instance in catalysis, biomedical applications, in inks and as composite materials. To ensure product quality and safe-by-design principles within the various application fields, the commercial material must be characterized and specified through well-known and standardized procedures. The accurate morphological characterization of 2D materials is a challenging task, requiring careful sample preparation on a substrate either as a powder or from liquid suspension. These must be isolated, homogeneously distributed, with good statistics of the counted particles. Various sample preparation approaches have been reported in the literature, e.g. electrospray, substrate surface treatment, embedding the particulate material and polishing the cross-section, or addition of ligands to the suspended nanostructures. In this study, a novel deposition procedure for graphene-related 2D materials (GR2Ms) was systematically tested for its efficacy. The quantitative analysis of the size and shape distribution of the materials was conducted using electron microscopy and was successfully tested in XPS and EDS experiments. The technique is an extension of the conventional drop-casting method and has been designated "wire-print" deposition. The result of such a wire-print deposition for a graphene-based suspension is shown in Figure, where various treatment conditions have been tested with a repetition of up to 10 times per condition, all together 86 spots on a silicon wafer of 10 mm². T2 - Graphene Week 2025 CY - Vicenza, Italy DA - 22.09.2025 KW - Graphene-related 2D materials (GR2M) KW - Sample peparation KW - Imaging KW - Electron Microscopy KW - Wire-print deposition method PY - 2025 AN - OPUS4-64248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Paun, I. A. A1 - Heitz, J. A1 - Stoian, R. T1 - Guest editorial: Making light matter N2 - This article represents the Guest Editorial of the Special Issue associated with the Symposium L "Making light matter: lasers in material sciences and photonics" held during the 2023 E-MRS Spring Meeting in Strasbourg, France, June 25th - July 2nd, 2023. T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - Guest Editorial KW - Laser KW - Material Science KW - Photonics PY - 2024 DO - https://doi.org/10.1002/pssa.202400528 SN - 1862-6319 VL - 221 IS - 15 SP - 1 EP - 5 PB - Wiley-VCH CY - Weinheim AN - OPUS4-60948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Florian, Camilo T1 - Optical thickness-profiling for fs-laserinduced superficial amorphization and oxide removal on silicon N2 - Amorphization and re-crystallization of polished silicon wafers cut in <111> and <100> orientation were studied after irradiation by single Ti:sapphire femtosecond laser pulses (790 nm, 30 fs) using optical imaging, topographic characterization, and transmission electron microscopy. Spectroscopic imaging ellipsometry (SIE) enabled fast data acquisition at multiple wavelengths and provided experimental data for calculating the amorphous layer thickness profiles with lateral resolution in the micrometer and vertical resolution in the nanometer range based on a thin-film layer model including the topmost native oxide. For a radially Gaussian shaped laser beam and at moderate peak laser fluences above the melting but below the ablation threshold, laterally parabolic amorphous layer profiles with maximum thicknesses of some tens of nanometers were quantitatively derived. Moreover, the threshold fluence of the native oxide removal was quantified. At laser peak fluences closely below the ablation threshold of silicon, SIE is capable to reveal even the laser-induced removal and formation of the native oxide covering the Si wafers under ambient air conditions. The accuracy of these all-optical, non-destructive SIE-based layer thickness assessments is verified experimentally through high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (STEM-EDX). Along with topographic information obtained by atomic force microscopy (AFM), a comprehensive picture of the oxide removal and superficial re-solidification of silicon after local melting by femtosecond laser pulses can be drawn. T2 - E-MRS Spring Meeting 2025 CY - Strasbourg, France DA - 26.05.2025 KW - Femtosecond laser KW - Laser-induced amorphization KW - Native oxide layer KW - Spectroscopic imaging ellipsometry KW - Transmission electron microscopy PY - 2025 AN - OPUS4-63275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Bacterial adhesion on ultrashort pulse laser processed surfaces ― more than size matters! N2 - Bacterial biofilms are aggregates of bacterial cells, often attached to a surface and enclosed by a self-produced extracellular matrix which confers increased stress tolerance and resistance to cleaning. Biofilm formation leads to biofouling which gives rise to high costs in numerous technical settings due to biocorrosion and biodegradation. However, biofilms can also be attractive for industrial settings such as wastewater treatment systems or for soil bioremediation processes. Hence, the control of bacterial adhesion to a surface is of major concern. Surface topography strongly influences bacterial adhesion. Therefore, one promising way to achieve bacteria-guiding surfaces lies in the contactless and aseptic large-area laser processing of technical surfaces. We used short and ultrashort pulsed laser systems to generate different surface textures, mainly high-spatial-frequency and low-spatial-frequency laser-induced periodic surface structures, LIPSS (HFSL and LFSL), on Ti, Ti-alloy, steel, and polymers (PET and PE). Pristine (polished) and laser processed samples were subjected to bacterial adhesion experiments with two different Escherichia coli strains and Staphylococcus aureus as test organisms. The bacterial strains differed in their cell wall structure (grampositive vs. gramnegative strains), in size, shape, the occurrence of cell appendages, and in their biofilm forming capabilities. Adhesion patterns were analyzed microscopically and compared regarding the respective test strain and surface topography. Our results revealed that adhesion behavior strongly depends not only on the material’s topography and chemistry, but also on the specific bacterial strain, the presence of cell appendages, and ambient growth conditions. T2 - 13th International Conference on Photoexcited Processes and Applications, ICPEPA-13 CY - Lecce, Italy DA - 14.09.2025 KW - Biofilm KW - Bacterial adhesion KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses PY - 2025 AN - OPUS4-64166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kaczmarek, D. A1 - Bonse, Jörn T1 - Capabilities and limitations of Sipe’s first principles LIPSS theory: current aspects and directions N2 - This presentation elucidates the fundamentals and capabilities of John E. Sipe’s first principles theory (1983) of laser-induced periodic surface structures (LIPSS), representing an analytical mathematical approach (Green’s formalism) to calculate the absorption of electromagnetic radiation at a microscopically rough surface via the so-called efficacy factor. It includes a discussion of assumptions made in the theory and resulting limitations, such as the restriction to a near-surface layer (the so-called “selvedge”), the lack of any material response, or missing inter-pulse feedback phenomena being relevant in typical multi-pulse irradiation conditions. The influence of the angle of incidence, the polarization direction (s-pol. or p-pol.), the optical properties (dielectric permittivity) of the irradiated materials, as well as its surface roughness and its specific encoding in the theory via a shape factor (s) and a filling factor (f) are addressed. A simplifying mathematical reformulation (without changing the validity range) of Sipe’s theory in the form of 14 complex-valued equations published in 2005 is motivated, as well as the necessity of some minor adjustments for non-normal incident radiation - revealed in a very recent Erratum. Starting with 2009, extensions of the original theory were developed, e.g., the analytical Sipe-Drude model in order to include intra-pulse transient changes of the optical properties of the material. Finite-difference time-domain (FDTD) numerical simulations successfully confirmed in 2012 the validity of the Sipe-Drude approach. Moreover, the FDTD formalism can be extended to sub-surface regions and can be combined with a material response (topography) modelling for iteratively considering inter-pulse feedback phenomena. Finally, we will provide characteristic examples of Sipe’s efficacy factor for typical material classes (metals, semiconductors, dielectrics), we will explain how the results can be interpreted, and line out how the Sipe theory may be extended further. T2 - 12th International LIPSS Workshop CY - Leipzig, Germany DA - 11.09.2024 KW - Laser-induced periodic surface structures (LIPSS) KW - Theory KW - Green's formalism KW - Scattering waves KW - Finite-difference time-domain calculations PY - 2024 AN - OPUS4-61098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martínez, E. A1 - Lejeune, N. A1 - Frechilla, J. A1 - Porta-Velilla, L. A1 - Forneau, E. A1 - Angurel, L. A. A1 - de la Fuente, G. F. A1 - Bonse, Jörn A1 - Silhanek, A. V. A1 - Badía-Majós, A. T1 - Laser engineered architectures for magnetic flux manipulation on superconducting Nb thin films N2 - Custom shaped magnetic flux guiding channels have been fabricated on superconducting Nb thin films by laser nanopatterning of their surface. Preferential pathways are defined by suitable combination of imprinted anisotropic pinning domains through laser-induced periodic surface structures (LIPSS). Generated by the selective energy deposition of femtosecond UV laser pulses, quasi-parallel ripple structures are formed under optimized irradiation conditions. On average, each domain is formed by grooves with a lateral period of 260–270 nm and a depth about 80 nm. By combination of scanning and transmission electron microscopy, magneto-optical imaging, and conductive atomic force microscopy techniques, we conclude that the boundaries of the LIPSS-covered domains play a prominent role in the magnetic flux diversion process within the film. This is confirmed by dedicated modeling of the flux dynamics, combined with the inversion of the magneto-optical signal. The created metasurfaces enable control of the flux penetration process at the microscale. KW - Laser-induced periodic surface structures (LIPSS) KW - Magnetic flux KW - Magneto-optical imaging (MOI) KW - Critical current density PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611243 UR - https://www.sciencedirect.com/science/article/pii/S0169433224019287 DO - https://doi.org/10.1016/j.apsusc.2024.161214 SN - 1873-5584 (Online) SN - 0169-4332 (Print) VL - 679 SP - 1 EP - 12 PB - Elsevier AN - OPUS4-61124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wonneberger, R. A1 - Gräf, S. A1 - Bonse, Jörn A1 - Wisniewski, W. A1 - Freiberg, K. A1 - Hafermann, M. A1 - Ronning, C. A1 - Müller, F. A. A1 - Undisz, A. T1 - Tracing the Formation of Femtosecond Laser-Induced Periodic Surface Structures (LIPSS) by Implanted Markers N2 - The generation of laser-induced periodic surface structures (LIPSS) using femtosecond lasers facilitates the engineering of material surfaces with tailored functional properties. Numerous aspects of their complex formation process are still under debate, despite intensive theoretical and experimental research in recent decades. This particularly concerns the challenge of verifying approaches based on electromagnetic effects or hydrodynamic processes by experiment. In the present study, a marker experiment is designed to conclude on the formation of LIPSS. Well-defined concentration depth profiles of 55Mn+- and 14N+-ions were generated below the polished surface of a cast Mn- and Si-free stainless steel AISI 316L using ion implantation. Before and after LIPSS generation, marker concentration depth profiles and the sample microstructure were evaluated by using transmission electron microscopy techniques. It is shown that LIPSS predominantly formed by material removal through locally varying ablation. Local melting and resolidification with the redistribution of the material occurred to a lesser extent. The experimental design gives quantitative access to the modulation depth with a nanometer resolution and is a promising approach for broader studies of the interactions of laser beams and material surfaces. Tracing LIPSS formation enables to unambiguously identify governing aspects, consequently guiding the path to improved processing regarding reproducibility, periodicity, and alignment. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser processing KW - Ion implantation KW - Transmission Electron Microscopy (TEM) KW - Stainless steel PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623990 DO - https://doi.org/10.1021/acsami.4c14777 SN - 1944-8244 (Print) SN - 1944-8252 (Online) VL - 17 IS - 1 SP - 2462 EP - 2468 PB - ACS Publications AN - OPUS4-62399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Laser Nanotexturierung von Metalloberflächen zur Reduktion von Reibung und Verschleiß N2 - Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nanostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet. T2 - Online Abendvortrag beim AWT Härterei- und Werkstoffkreis Bodensee der Arbeitsgemeinschaft Wärmebehandlung + Werkstofftechnik e.V. CY - Online meeting DA - 16.01.2025 KW - Additive KW - Laser-induzierte periodische Nanostrukturen KW - Reibungsreduktion KW - Verschleißreduktion PY - 2025 AN - OPUS4-62432 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - Morphology and regularity of high-spatial frequency laser-induced periodic surface structures (HSFL) on titanium materials N2 - Titanium and its alloys are known to allow the straightforward laser‐based manufacturing of ordered surface nanostructures, so‐called high spatial frequency laser‐induced periodic surface structures (HSFL). These structures exhibit sub‐100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, HSFL were processed on different titanium materials (bulk, film) upon irradiation with near‐infrared ps‐laser pulses (1030 nm wavelength, ≈ 1 ps pulse duration) under different laser scan processing conditions. Here we extend our previous work on chemical analyses of HSFL on titanium materials towards a more detailed morphological and topographical surface characterization. For that, scanning electron and atomic force microscopic images are subjected to a regularity analysis using our self-developed ReguΛarity software. The regularity of the HSFL is assessed with respect to the influences of sample- and laser-related parameters, as well as the imaging method used. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Titanium KW - Ultrashort laser pulses KW - Laser processing PY - 2025 AN - OPUS4-64631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Laser Nanotexturierung von Metalloberflächen zur Reduktion von Reibung und Verschleiß N2 - Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nanostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet. T2 - Internationale Bodensee Fachtagung „Wärmebehandlung und Oberflächentechnik zur Verbesserung von Tribologie und Verschleissbeständigkeit" CY - Feldkirch, Austria DA - 20.03.2025 KW - Additive KW - Laser-induzierte periodische Nanostrukturen KW - Reibungsreduktion KW - Verschleißreduktion PY - 2025 AN - OPUS4-62757 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Generation and characterization of anisotropic nanostructures using ultrashort pulsed lasers N2 - The lecture gives an overview of the generation and characterization of anisotropic nanostructures using ultrashort pulsed laser radiation. Special attention will be paid to the phenomenon of so-called laser-induced periodic surface structures (LIPSS) on various materials. One focus will be on dielectrics and the dynamics of nanostructure formation. Further examples of bulk nanostructures from the literature will be discussed. T2 - 8th UKP-Workshop: Ultrafast Laser Technology CY - Aachen, Germany DA - 08.04.2025 KW - Laser-induced Periodic Surface Structures (LIPSS) KW - Dielectrics KW - Surface Nanostructures KW - Volume Nanostructures PY - 2025 AN - OPUS4-62947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Bonse, Jörn ED - Paun, I. A. ED - Heitz, J. ED - Stoian, R. T1 - Special issue: Making light matter N2 - This special issue represents the proceedings of the Symposium L "Making light matter: lasers in material sciences and photonics" held from May 29th to June 2nd 2023 in Strasbourg, France, during the 2023 Spring Meeting of the European MaterialsResearch Society (E-MRS). T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - E-MRS Spring Meeting 2023 KW - Laser Processing KW - Material Science KW - Photonics PY - 2024 UR - https://onlinelibrary.wiley.com/toc/18626319/2024/221/15 SN - 1862-6319 VL - 221 IS - 15 SP - 2300478 EP - 2400528 PB - Wiley-VCH CY - Weinheim AN - OPUS4-60949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Ultrafast optical probing of laser-induced formation of periodic surface nanostructures N2 - Laser-induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any type of solid upon irradiation with intense laser pulses. They represent a (quasi-)periodic modulation of the surface topography in the form of a linear grating and are typically formed in a “self-ordered” way in the focus of a coherent laser beam. Thus, they are often accompanying laser material processing applications. The structural sizes of LIPSS typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, a controversial debate has emerged during the last decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter-reorganization processes (distinctly after the laser irradiation). From a practical point of view, however, LIPSS represent a simple and robust way for the nanostructuring of solids that allows creating a wide range of different surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. The presentation provides an overview of current theories on LIPSS and the quest to achieve ever smaller surface nanostructures. The historical development of the fundamental ideas behind LIPSS is presented, together with experimental approaches that make it possible to distinguish between the various LIPSS formation scenarios. Time-resolved experimental methods are required to investigate the dynamics of their formation. The presentation focuses on ultrafast time-resolved optical (pump-probe) techniques that can be used for localized point measurements or microscopic imaging, utilizing the reflection, diffraction, or coherent scattering of the probe radiation at the emerging LIPSS, while simultaneously capturing information about rapid melting, ablation, and solidification phenomena. However, given the sub-micrometric spatial periods of LIPSS, their analysis using optical radiation employed in far-field techniques remained a challenge. Therefore, short wavelengths of the probe beam in the UV range or even below are required to overcome the diffraction limit imposed in the optical spectral range. Fourth-generation light sources, namely short-wavelength (XUV or X-ray) short-pulse free-electron lasers (FELs), offer new and fascinating possibilities for resolving laser-induced structure formation on surfaces in the sub-micrometer to nanometer range and in time domains from picoseconds to several nanoseconds with a resolution in the sub-picosecond regime. On laser-irradiated semiconductor surfaces, this unique spatio-temporal resolution enables the detection of early signs of coherent/plasmonic electromagnetic scattering effects, followed by the excitation of hydrodynamic capillary waves – providing new insights into the above-mentioned debate. Recent experiments at the European XFEL used fs-time-resolved small-angle X-ray scattering (fs-SAXS) and even fs-time-resolved grazing incidence small-angle X-ray scattering (fs-GISAXS), combined with grazing-incidence diffraction (fs-GID), to reveal the dynamics of the formation of nanometric LIPSS on metals. T2 - CINSaT Herbstkolloquium 2025 CY - Kassel, Germany DA - 05.11.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses KW - Pump-probe measurements KW - Free-electron laser KW - Small angle X-ray scattering (SAXS) PY - 2025 AN - OPUS4-64633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hassenstein, Christian T1 - Robotergestützte Ultraschallprüfung von Objekten mit komplexen Geometrien N2 - Durch den Einsatz moderner digitaler Design- und Fertigungsmethoden wachsen einerseits die Komplexität von Bauteilen, andererseits der Bedarf an Informationen über deren Qualität und Zustand. Damit steigen auch die Anforderungen an die zerstörungsfreie Prüfung, die im Zuge von ZfP 4.0 automatisierte und flexible, innovative Prüfmethoden erfordert. Das gilt insbesondere für Objekte, deren Oberflächengeometrien über plane Flächen und eindimensionale Krümmungen hinausgehen. Um zu zeigen, wie eine Ultraschallprüfung von Objekten mit komplexer Oberflächengeometrie realisiert werden kann, wurde an der BAM eine roboterbasierte Demonstratoranlage entwickelt. Dabei führt ein Roboterarm einen Array-Prüfkopf in Tauchtechnik senkrecht über die Prüffläche. Die dafür erforderliche Prüfbahn kann entweder anhand der CAD-Geometrie oder mithilfe einer Punktewolke der Prüffläche, die vorab mit einem am Roboter angebrachten Laser-Profilometer erfasst wird, ermittelt werden. Zur Erhöhung der Genauigkeit werden der Lasersensor und der Ultraschallprüfkopf automatisiert mit dafür entwickelten Routinen am Roboter eingemessen. Durch bildgebende Verfahren und eine automatische Auswertung der Bilder kann die in Tauchtechnik auftretende Brechung des Schallbündels an der Prüfteiloberfläche berücksichtigt werden, was die ortsrichtige Rekonstruktion von Anzeigen aus dem Prüfteilinneren bzw. der Rückwand ermöglicht. Durch Rückführung der Anzeigen in ein gemeinsames Koordinatensystem entsteht eine 3D-Rekonstruktion des Prüfteils. Der vorliegende Beitrag stellt die Demonstratoranlage und die angewendeten Methoden im Detail vor und nennt Anwendungsbeispiele. T2 - DGZfP Jahrestagung 2025 CY - Berlin, Germany DA - 26.05.2025 KW - Ultraschall KW - Robotik KW - Turbinenschaufel KW - Wanddicke KW - Defekterkennung PY - 2025 AN - OPUS4-63417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - ReguΛarity - A free software for the objective quantification of the regularity of periodic surface structures generated by femtosecond laser irradiation N2 - The precise laser-based surface structuring on the micro- and nanoscale allows to create functional properties for innovative applications, e.g., in medicine, optics and biology. Among the various types of surface structures, laser-induced periodic surface structures (LIPSS) are characterized by their versatility and the relatively simple manufacturing process. However, the fabrication of highly regular LIPSS patterns remains challenging. The systematic investigation of LIPSS formation, as well as of the resulting functional properties requires a precise evaluation of the surface morphology, especially with regard to periodicity and regularity. Existing quantification methods such as Fast Fourier Transformation (FFT) tend to lack automation and objectivity, especially when dealing with large data sets and multi-scale structures. Although automated approaches exist with the Gini coefficient and the P³S method, their limited availability restricts a broader scientific use. We therefore introduce ReguΛarity as an innovative open-source software solution for objective, rapid and reproducible evaluation of structured surfaces concerning their regularity. In order to provide comprehensive surface morphological analysis, our software uses advanced image-processing techniques and integrates the already developed tools such as P³S method, Gini coefficient, FFT analysis, and the calculation of DLOA (Dispersion of LIPSS Orientation Angle). The software allows to evaluate any relevant image format as provided, e.g., by standard scanning electron micrographs. An intuitive PyQt5-based interface, enhanced by multi-threading capabilities, facilitates efficient data processing. Interactive features such as region-of-interest selection and plotting provide flexible adaptation to diverse applications. ReguΛarity offers a robust analysis tool that will contribute to the further development of precise laser-based surface structuring and to the optimization of the desired functional properties in both research and industry. T2 - 13th International Conference on Photoexcited Processes and Applications, ICPEPA-13 CY - Lecce, Italy DA - 14.09.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Laser processing KW - Fourier transformation KW - Regularity PY - 2025 AN - OPUS4-64176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rahner, E. T1 - From nightmare to numbers - A novel software tool for objective regularity analysis of LIPSS N2 - The precise laser-based surface structuring on the micro- and nanoscale allows for the creation of functional properties for innovative applications, e.g., in medicine, optics and biology. Among the various types of surface structures, laser-induced periodic surface structures (LIPSS) are distinguished by their versatility and the comparatively simple manufacturing process. Nevertheless, the fabrication of highly regular LIPSS patterns remains challenging. The systematic investigation of LIPSS formation, as well as of the resulting functional properties demands accurate and objective evaluation of surface morphology, especially regarding periodicity and regularity. Existing quantification methods such as Fast Fourier Transformation (FFT) tend to lack automation and objectivity, especially when dealing with large data sets and multi-scale structures. Although automated approaches, such as those based on the Gini coefficient or the P³S method, have been proposed, their limited availability hinders a broader scientific use. To overcome these limitations, we introduce ReguΛarity, a novel, freely available Python-based software tool featuring a graphical user interface for automated and quantitative assessment of regularity in period and (quasi-)periodic surface patterns including LIPSS. The software processes microscopic images obtained from optical, scanning electron microscopy (SEM), or atomic force microscopy (AFM), combining image segmentation with one- and two-dimensional Fourier analyses (1D-FT, 2D-FT), phase evaluation, and gradient-based orientation determination to facilitate a comprehensive regularity analysis of (quasi-)periodic surface patterns with spatial periods Λ. Regularity is quantified by the newly proposed five-dimensional regularity tuple R comprising the normalized spread of spatial periods from 2D-FT, the normalized local variation of the dominant spatial period from 1D-FT, the Gini coefficient G, the Dispersion of the LIPSS Orientation Angle (DLOA), and the mean phase deviation. The demonstration of the software’s capabilities is achieved by comparing idealized sinusoidal test patterns with SEM micrographs of fs-laser-generated LIPSS on stainless steel (AISI 316L) and aluminum alloy (AlMg5). This comparison highlights ReguΛarity’s objective differentiation between varying levels of structural regularity. The software facilitates high-throughput analysis and data-driven optimization in laser surface engineering processes. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - Fourier transform KW - Gini coefficient PY - 2025 AN - OPUS4-65047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gräf, S. T1 - Ion marker implantation as key to understand the formation of femtosecond LIPSS on steel N2 - Ultrashort laser (fs-laser) pulses can be used to generate laser-induced periodic surface structures (LIPSS, ripples) on different types of materials. A variety of potential applications of these grating-like LIPSS have already been demonstrated in the field of surface functionalization. Examples include structural colours (e.g. for optical effects or safety features), beneficial friction and wear reduction, modification of the wetting behaviour of surfaces, and antibacterial or cell adhesion promoting properties for medical implants. Despite decades of research, however, some aspects regarding the formation mechanism are still unclear and the subject of controversial debate. This involves the two main models of coherent electromagnetic scattering and matter reorganization, which are used for explaining aspects of LIPSS formation and phenomenology. One major issue is to quantify the actual amount of material removal during the fs-laser processing due to the lack of an independent depth reference and to visualize the so-called heat-affected zone accompanying intense fs-laser irradiation. In the present study, near-surface implantation of Mn and N ions into different material depth of Mn-free austenitic stainless steel alloy FeCrNiMo18-12-2 was used to create reference layers of a defined thickness containing the respective elements. LIPSS (type low-spatial frequency LIPSS, LSFL) were fabricated on the polished substrate surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz, F = 1.5 J/cm2). The implanted layers subsequently served as a kind of coordinate system to assess the material removal during the formation process via cross-sectional Transmission Electron Microscopy (TEM) and Energy Dispersive X-ray Spectroscopy (EDXS). Using both analysis methods enabled in particular to determine the position of peaks and valleys of the LIPSS topography in relation to the initial surface before fs-laser irradiation. This confirmed the selective ablation in the LIPSS valleys. Moreover, linking changes in the material’s microstructure, e.g., the crystallinity and near surface elemental composition before and after fs-laser treatment, gave additional insights regarding the transient cooling rates, as recently shown for NiTi alloys. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2015 KW - Energy dispersive X-ray analysis (EDX) KW - Ion implantation KW - Laser-induced periodic surface structures (LIPSS) KW - Steel KW - Transmission electron microscopy (TEM) PY - 2025 AN - OPUS4-64900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Bacterial adhesion on ultrashort pulse laser processed surfaces ― more than size matters! N2 - Bacterial biofilms are aggregates of bacterial cells, often attached to a surface, and enclosed by a self-produced extracellular matrix which confers increased stress tolerance and resistance to cleaning. Biofilm formation leads to biofouling which gives rise to high costs in numerous technical settings due to biocorrosion and biodegradation. However, biofilms can also be attractive for industrial settings such as wastewater treatment systems or for soil bioremediation processes. Hence, the control of bacterial adhesion to a surface is of major concern. Surface topography strongly influences bacterial adhesion. Therefore, one promising way to achieve bacteria-guiding surfaces lies in the contactless and aseptic large-area laser processing of technical surfaces. We used short and ultrashort pulsed laser systems to generate different surface textures, mainly high-spatial-frequency and low-spatial-frequency laser-induced periodic surface structures, LIPSS (HFSL and LFSL), on Ti, Ti-alloy, steel, and polymers (PET and PE). Pristine (polished) and laser processed samples were subjected to bacterial adhesion experiments with two different Escherichia coli strains and Staphylococcus aureus as test organisms. The bacterial strains differed in their cell wall structure (grampositive vs. gramnegative strains), in size, shape, the occurrence of cell appendages, and in their biofilm forming capabilities. Adhesion patterns were analyzed microscopically and compared regarding the respective test strain and surface topography. Our results revealed that adhesion behavior strongly depends not only on the material’s topography and chemistry, but also on the specific bacterial strain, the presence of cell appendages, and ambient growth conditions. T2 - 13th International LIPSS Workshop CY - Enschede, Netherlands DA - 29.10.2025 KW - Bacterial adhesion KW - Biofilm KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses PY - 2025 AN - OPUS4-64632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voss, Heike T1 - Morphology and regularity of high-spatial frequency laser-induced periodic surface structures (HSFL) on titanium materials N2 - Titanium and its alloys are known to enable the straightforward laser‐based manufacturing of ordered surface nanostructures, so‐called high-spatial frequency laser‐induced periodic surface structures (HSFL). These structures exhibit sub‐100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, HSFL were processed on different titanium materials (bulk, film) upon irradiation with near‐infrared ps‐laser pulses (1030 nm wavelength, ≈1 ps pulse duration) under different laser scan processing conditions in normal air atmosphere. Here, we extend our previous work on chemical analyses of HSFL on titanium materials towards a more detailed large-area morphological and topographical surface characterization. For this purpose, scanning electron or atomic force microscopic images are subjected to a regularity analysis using our ReguΛarity software. The results are assessed with respect to the influences of sample- or laser-related parameters on the regularity of the HSFL. T2 - 13th International Conference on Photoexcited Processes and Applications, ICPEPA-13 CY - Lecce, Italy DA - 14.09.2025 KW - Laser-induced periodic surface structures (LIPSS) KW - Laser processing KW - Ulltrashort laser pulses KW - Titanium PY - 2025 AN - OPUS4-64173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gräf, S. T1 - Ion marker implantation for tracing the formation of femtosecond LIPSS on steel N2 - An ion marker experiment is conducted to investigate the formation of low spatial frequency laser-induced periodic surface structures (LIPSS) on stainless steel surfaces upon scan-processing with femtosecond laser pulses (300 fs, 1025 nm, 100 kHz) focussed to a spot diameter of ~20 µm. Defined concentration depth profiles of 14N^+- and 55Mn^+-ions were implanted below the polished surface of a cast Mn- and Si-free stainless steel AISI 316L using an acceleration energy of 380 keV. This generated two distinct “depth-tracer-layers” ~135 nm (55Mn) and ~340 nm (14N) below the sample surface. The sample morphology and microstructure were evaluated before and after LIPSS-processing using scanning and transmission electron microscopy techniques in top-view and cross-sectional geometry. Energy-dispersive X-ray spectroscopy (EDXS) allowed to visualize the depth distribution of the marker elements, the steel constituents, and of oxygen involved through the laser processing in ambient air. These experiments revealed that the LIPSS on this metal are predominantly formed by material removal through locally varying ablation and, to a lesser extent, by local melt displacement effects prior to the re-solidification. Moreover, the processing in air leads to the formation of a less than 10 nm thick laser-induced oxide layer covering the steel surface. Our new tracer ion approach contributes to the ongoing debate on the relevance of electromagnetic or hydrodynamic effects during the formation of LIPSS. T2 - E-MRS Spring Meeting 2025 CY - Strasbourg, France DA - 26.05.2026 KW - Laser-induced periodic surface structures (LIPSS) KW - Steel KW - Ion implantation KW - Transmission electron microscopy (TEM) KW - Energy dispersive X-ray analysis (EDX) PY - 2025 AN - OPUS4-63274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - MINERVA-OS: The Orchestrator of our SDL for Nano and Advanced Materials Synthesis N2 - We present our SDL "Minerva" and its' Orchestrator "Minerva-OS". We discuss the general architecture of the orchestrator, the problems our orchestration solution solves, associated objectives, and success criteria. We demonstrate how a user would interact with it and give examples of what it has already been used for. We also provide some explanation of the available and planned features, and how workflows/experiments are represented. Lastly, we discuss key technical challenges we faced during development. T2 - Orchestration Alignment Virtual Workshop CY - Online meeting DA - 20.01.2026 KW - Self Driving Labs KW - Materials Acceleration Platforms KW - Workflows KW - Orchestration PY - 2026 AN - OPUS4-65422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Ein seltener mononuklearer Lithium‐Carben‐Komplex für die Atomlagenabscheidung von lithiumhaltigen Dünnschichten N2 - KurzfassungLithium ist das zentrale Element moderner Batterietechnologien, und die Herstellung von lithiumhaltigen Materialien mittels Atomlagenabscheidung (engl. Atomic Layer Deposition, ALD) bietet erhebliche Vorteile bei der Kontrolle der Schichtdicke und ‐zusammensetzung. In dieser Studie wird ein neuer mononuklearer, durch ein N‐heterocyclisches Carben (NHC) stabilisierter Lithiumkomplex, [Li(tBuNHC)(hmds)], als vielversprechender Präkursor für die ALD von lithiumhaltigen Dünnschichten vorgestellt. Die strukturelle Charakterisierung erfolgt durch den Vergleich von Dichtefunktionaltheorie (DFT) und Einkristall‐Röntgenbeugung (engl. Single‐Crystal X‐ray Diffraction, SC‐XRD), wobei die seltene mononukleare Struktur bestätigt wird. Thermogravimetrische Analysen (TGA) zeigen vorteilhafte thermische Eigenschaften für ALD‐Anwendungen. Die Verbindung weist einen niedrigen Schmelzpunkt, saubere Verdampfung und ermutigende Volatilitätsparameter im Vergleich zu anderen Lithium‐Präkursoren auf. ALD‐Experimente mit [Li(tBuNHC)(hmds)] und Ozon zeigen dessen Effektivität bei der Abscheidung von LiSixOy‐Filmen. Der ALD‐Prozess zeigt ein gesättigtes Wachstum pro Zyklus (engl. Growth per Cycle, GPC) von 0,95 Å. Die Zusammensetzung, analysiert mittels Rutherford‐Rückstreu‐Spektrometrie/Kernreaktionsanalyse (engl. Rutherford Backscattering Spectrometry/Nuclear Reaction Analysis, RBS/NRA), Röntgenphotoelektronenspektroskopie (engl. X‐ray Photoelectron Spectroscopy, XPS) und Glimmentladungsspektroskopie (engl. Glow Discharge Optical Emission Spectrometry, GD‐OES), bestätigt das Vorhandensein von Lithium und Silizium in den erwarteten Verhältnissen. Diese Arbeit stellt nicht nur einen neuen ALD‐Präkursor vor, sondern trägt auch zum Verständnis der Lithiumchemie bei und bietet Einblicke in die faszinierende Koordinationschemie und das thermische Verhalten von durch NHC‐Liganden stabilisierten Lithiumkomplexen. KW - Atomlagenabscheidung KW - N-heterozyklischer-Carben-(NHC)-stabilisierter Lithium-Präkursor KW - Mononuklearer Li–Carben-Komplex KW - Lithiumsilicat-Dünnfilme KW - Filmanalytik/-Charakterisierung PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644045 DO - https://doi.org/10.1002/ange.202513066 SN - 0044-8249 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier SP - 1 EP - 12 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64404 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad Andrade, Carlos Enrique A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Rare Mononuclear Lithium-Carbene Complex for Atomic Layer Deposition of Lithium Containing Thin Films N2 - Lithium is the core material of modern battery technologies and fabricating the lithium‐containing materials with atomic layer deposition (ALD) confers significant benefits in control of film composition and thickness. In this work, a new mononuclear N‐heterocyclic carbene (NHC) stabilized lithium complex, [Li(tBuNHC)(hmds)], is introduced as a promising precursor for ALD of lithium‐containing thin films. Structural characterization is performed, comparing density functional theory (DFT) and single‐crystal X‐ray diffraction (SC‐XRD), confirming a rare mononuclear structure. Favorable thermal properties for ALD applications are evidenced by thermogravimetric analysis (TGA). The compound exhibits a low melting point, clean evaporation, and its volatility parameters are encouraging compared to other lithium precursors. ALD trials using [Li(tBuNHC)(hmds)] with ozone demonstrate its effectiveness in depositing LiSixOy films. The ALD process exhibits a saturated growth per cycle (GPC) of 0.95 Å. Compositional analysis using Rutherford backscattering spectrometry/nuclear reaction analysis (RBS/NRA), X‐ray photoelectron spectrometry (XPS), and glow discharge optical emission spectrometry (GD‐OES), confirms the presence of lithium and silicon in the expected ratios. This work not only presents a new ALD precursor but also contributes to the understanding of lithium chemistry, offering insights into the intriguing coordination chemistry and thermal behavior of lithium complexes stabilized by NHC ligands. KW - Atomic layer deposition (ALD) KW - N-heterocyclic carbene (NHC) ligands KW - Lithium ALD precursor chemistry KW - Mononuclear Li–carbene complex [Li(tBuNHC)(hmds)] KW - Li-silicate thin films (LiSixOy) KW - Thermal properties & TGA/volatility KW - Compositional analysis (RBS/NRA, XPS, GD-OES) PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643790 DO - https://doi.org/10.1002/anie.202513066 SN - 1433-7851 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Campos de Oliveira, Paula T1 - Advancing microstructural characterisation of ceramic cores for aerospace: from state-of-the-art to in-situ synchrotron X-ray computed tomography N2 - Ceramic cores are crucial for manufacturing turbine blades in aircraft engines, creating intricate cooling channels that improve engine efficiency and reduce emissions. During high-temperature casting, the cores undergo significant microstructural changes, including phase transitions, particle rearrangements, and porosity transformations, which can affect their properties and must be carefully controlled. State-of-the-art characterisation techniques for ceramic cores mostly rely on 2D methods, such as scanning and transmission electron microscopy. While valuable, these methods are limited in capturing the 3D complexity of the material. Advances in X-ray computed tomography (XCT) offer a more comprehensive perspective on 3D microstructures, but conventional XCT often lacks the resolution and in-situ capabilities to study microstructural evolution under casting conditions. Synchrotron XCT (SXCT) addresses these limitations, offering high spatial and temporal resolution with features down to 1 µm, enabling in-situ investigations. This study highlights the potential of SXCT, revealing previously unseen 3D microstructural features in ceramic cores, such as agglomeration, porosity evolution, surface reactions, microcracking, and particle orientation. These findings provide a more realistic view of dynamic changes during casting, advancing the understanding of core behaviour. Despite its advantages, SXCT is still rarely used in the field due to challenges such as limited access to synchrotron facilities and sample movement artifacts. Future developments, including high-temperature and vacuum compatible CT setups, could enhance this technique, leading to a better optimisation of ceramics performance. T2 - XIXth Conference of the European Ceramic Society (ECERS 2025) CY - Dresden, Germany DA - 31.08.2025 KW - Synchrotron KW - X-ray Computed Tomography KW - Ceramic core KW - Aerospace KW - Microstructure PY - 2025 AN - OPUS4-64050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Onyenso, Gabriel A1 - AI-Zawity, Jiwar A1 - Farahbakhsh, Nastaran A1 - Schardt, Annika A1 - Yadigarli, Aydan A1 - Vakamulla Raghu, Swathi Naidu A1 - Engelhard, Carsten A1 - Müller, Mareike A1 - Schönherr, Holger A1 - Killian, Manuela S. T1 - Novel Ag-modified zirconia nanomaterials with antibacterial activity N2 - The outcome of an implant procedure largely depends on the implant's surface properties. Biomaterials are now designed to have surfaces with multifunctionality, such as favorable tissue integration and the ability to combat bacterial adhesion and colonization. Herein, we report on a simple approach to improve the antibacterial properties of zirconia nanotubes (ZrNTs) coatings by decorating with silver nanoparticles (AgNP), achieved through electrochemical anodization of a zirconium–silver alloy (Zr–Ag). The AgNPs were shown to partially consist of Ag2O, potentially enhancing the availability of Ag+ ions for antibacterial activity. The modified ZrNTs were characterized using SEM, EDS, ToF-SIMS, and XPS to determine their structural morphology and chemical composition, and were further subjected to antibacterial testing. The silver and zirconium ion release behavior was monitored via ICP-MS. ZrNTs decorated with AgNP exhibit strong antimicrobial activity (>99% bacterial killing) against both S. aureus and E. coli. Antimicrobial tests indicate that the antibacterial activity against the Gram-positive pathogen S. aureus was improved by a factor of 100 compared to unmodified ZrNTs, while unmodified ZrNTs already showed a comparable reduction of viable Gram-negative E. coli. This strategy illustrates a straightforward and effective modification that optimizes the interface between the host environment and the biomaterial surface to meet the very important criteria of biocompatibility and active antibacterial response. KW - Mass Spectrometry KW - Nanoparticles KW - Advanced Materials KW - ICP-MS KW - Antimicrobial material KW - ToF-SIMS PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653990 DO - https://doi.org/10.1039/d5ra07099f SN - 2046-2069 VL - 16 IS - 3 SP - 2286 EP - 2297 PB - Royal Society of Chemistry (RSC) AN - OPUS4-65399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Stoian, R. A1 - Bonse, Jörn T1 - Ultrafast Laser Nanostructuring — The Pursuit of Extreme Scales N2 - Long seen as “a solution seeking a problem,” laser pulses are nowadays – more than 60 years after their first practical demonstration – paramount in shaping and structuring matter. Harnessing their capabilities to direct intense beams of light, the number of scientific and technological developments and daily-life applications is continuously increasing. Today, the presence of lasers is ubiquitous in all sites of scientific and technological interest, from the most advanced research laboratories to industrial factories and medical hospitals. The directionality of the laser beam determines equally a local character on lightmatter interaction and as such a local modification to a material target. Furthermore, the coherence of laser radiation enables near-field or far-field scattering and interference effects that widen significantly the capabilities of controlling and tracking laser-matter interactions in space and time. Already with the advent of lasers, powerful beams of light have been directed at solid materials for a variety of purposes, making this application as old as the laser itself. The roots of the major applications for laser structuring were developed already in the 1960s, setting the base of both theoretical and experimental studies on laser ablation, with the number of publications expanding explosively during the next decades. Within this dynamic context, laser processing of materials experienced an impressive development over the years. Laser processing means specifically the capability to structure and tailor a material on its surface or even within its volume, rendering new functions and properties that are impacting the mechanical, electrical, or optical characteristics of the material. These properties are scaledependent, generating thus over the years an equally impressive quest for spatial or temporal resolution. Therefore, the developments in laser engineering with major breakthroughs, notably in pulse duration and power, always closely accompanied the efforts in material structuring with two milestones in sight: (1) yield and (2) resolution. Every step in shrinking the laser pulse duration led to a subsequent strong-impact development in process precision – particularly when the ultrashort pulse durations surpassed the fundamental electron-phonon relaxation times. Thus, minimizing heat diffusion, the advent of pulses with duration smaller than molecular or lattice vibration times has managed to confine the spatial resolution to the optical diffraction limit and sometimes even beyond. The nanoscale was already in sight at the turn of the millennium. An important question may be raised now; is there any fundamental limit in the processing resolution, a barrier defined by the intrinsic properties of light and matter? The answer has an inherently multidisciplinary nature, following the conversion of free-propagating electromagnetic radiation into material-confined energy potentially usable to drive or transform matter, and will be the focus of the present book. Relying on the experience and expertise of the leading researchers in the field, the present book intends to explore the current efforts in achieving laser processing resolution beyond the diffraction limit, laying down a perspective towards extreme laser nanostructuring. Following the most recent advances and developments, it puts forward a concept of extreme processing scales enabled by optical pulses that are able to bypass diffraction limits and achieve structuring characteristic scales beyond 100 nm. This objective can be achieved by a comprehensive understanding on how light can change matter and how, in turn, matter can change light, allowing jointly for actively controlling light and material processes. In order to give an extended perspective on the current state-of-the-art in the field of precision laser structuring, the book is divided into three main parts. The first part of the book (Part I: Fundamental Processes) offers a perspective into the fundamentals of laser-matter interaction on extreme spatial scales, with a description of the most advanced modeling efforts in understanding energy deposition in matter, a plethora of material-relaxation pathways, as well as advanced concepts for probing and observing matter in motion. Roadmaps for energy localization will be developed, and the atomistic perspective of laser ablation visualized. Theoretical modelling enables in-depth insights on ultrafast quantum processes at the nanoscale. Laser-driven self-organization at surfaces will be dissected regarding the question of how light drives material periodic patterns down to the nanoscale, explored and transmitted to its ultimate limits of an atomic printer, and immediately complemented by the unprecedented capabilities of ultrafast in-situ observation approaches for tracking the laser-induced material response with extreme spatial and temporal resolution. In the second part of the book (Part II: Concepts of Extreme Nanostructuring), distinct concepts will be developed and explored that allow confinement of light and harnessing of a material response restricted to nano- or mesoscopic scales at surfaces or in the volume of irradiated materials. A special focus will be on optical near-field related approaches for localizing light on scales even below the optical diffraction limit and plasmonic printing. Spatial and temporal beam-shaping and tailored interference techniques are discussed in the context of ultrashort laser pulses, and insights into some extreme states of matter realized by the tight confinement of laser energy are presented. The ultimate limits of writing waveguides in the bulk of dielectrics and for manifesting 3D-nanolithography are elucidated. Plasma-based surface treatments can significantly enhance the vertical precision of surface processing through etching processes. Finally, the third part of the book (Part III: Applications) leads us to a number of resuming applications, unveiling the tremendous capabilities of surface functionalization through laser micro- and nanostructuring, assessing the 3D-writing of waveguides in the bulk of dielectrics or semiconductors for enabling new branches of integrated photonics, and summarizing related applications ranging from nanophotonics to nanofluidics and from optical sensing to biomedical applications, including the latest capabilities of refractive eye surgery. This part will analyze the applications’ compatibility in yield and reproducibility with current industrial requirements, costs, and intellectual property aspects. It expands the involved spatial scales by more than eight orders of magnitude, when extending extremely small structures featuring sizes of few tens of nanometers to larger dimensions in the meter range. Thus, from surfaces to the bulk, from subtractive to additive manufacturing approaches, from advanced theoretical frames to practical technological processes – we invite the readers here to an exciting journey into the varicolored landscape of extreme laser nanostructuring. The idea of this book project was seeded in early 2020. We were delighted about the numerous and extremely positive responses from the laser-processing community, quickly receiving commitments for more than 30 individual book chapters. About 2500 communications later, the book is published. We would like to thank all authors of this book project for their insightful and detailed chapters, reviewing and reporting on this fascinating topic of the pursuit of extreme scales in ultrafast laser nanostructuring. Moreover, we would like to acknowledge the professional help and guidance of the staff of Springer Nature. Finally, we hope you will enjoy reading this book as much as we have enjoyed putting it together. Saint Etienne, France Razvan Stoian Berlin, Germany Jörn Bonse December 2022 KW - Laser nanostructuring KW - Surface engineering KW - Nonlinear lithography KW - Self-organization KW - Laser-induced periodic surface structures, LIPSS PY - 2023 SN - 978-3-031-14752-4 SN - 978-3-031-14751-7 DO - https://doi.org/10.1007/978-3-031-14752-4 SN - 0342-4111 VL - 239 SP - 1 EP - 1245 PB - Springer Nature Switzerland AG CY - Cham ET - 1 AN - OPUS4-57294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hörenz, Christoph A1 - Tache, O. A1 - Bartczak, D. A1 - Nunez, S. A1 - Abad Alvaro, I. A1 - Goenaga-Infante, H. A1 - Hodoroaba, Vasile-Dan T1 - A Study on the Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Electron Microscopy N2 - The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles. KW - Nanoparticles KW - Particle size distribution KW - Bimodal size distribution KW - Traceability PY - 2020 DO - https://doi.org/10.1017/S1431927620021054 VL - 26 IS - S2 SP - 2282 EP - 2283 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - Various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM are presented. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Particle size distribution KW - Sample peparation KW - Electron microscopy PY - 2020 AN - OPUS4-51716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria A1 - Hodoroaba, Vasile-Dan T1 - Project 15 Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension N2 - The progress in the VAMAS Project #15" Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension" within TWA 34 Nanoparticle Populations is presented with highlight of the following points: - Determine and compare particle size and shape distribution by means of: • electron microscopy (SEM, TEM, STEM-in-SEM) • atomic force microscopy (AFM) • small angle X-ray scattering (SAXS) - Determine uncertainty induced by deposition protocol from liquid suspension with comparison to known values from a prior ILC with already deposited nanoparticles on TEM grids. - Provide comparative validation of protocols for the techniques other than TEM. T2 - VAMAS Regional Workshop 2023 CY - Online meeting DA - 24.01.2023 KW - Nanoparticles KW - VAMAS KW - Electron microscopy KW - AFM KW - SAXS KW - TiO2 PY - 2023 UR - https://www.bam.de/Content/EN/Events/2023/2023-01-24-vamas-regional-workshop.html AN - OPUS4-57220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Morphological Analysis of Graphene Oxide by SEM and Correlative Field-Flow Fractionation Coupled with Multi-Angle Light Scattering N2 - Since the first free-standing monolayer graphene sheet was successfully prepared in 2004 [1], graphene and graphene oxide materials achieved the necessary technical readiness level to be considered for use in commercial products. Moreover, the focus has shifted from fundamental research towards expanding the applicability of graphene-related 2D materials (GR2M) and to improve their competitiveness with established materials [2]. Significant advances have been made especially in applications regarding optoelectronics, energy storage materials, chemical additives, sensor applications etc. [3]. Composite products containing graphene and functionalized graphene such as inks and dyes have shown enhanced performance regarding longevity, wettability, and can be tailored for specific purposes through dedicated functionalization. For accurate physico-chemical characterization, GR2M products in their raw form or as part of composites present challenges in terms of sample preparation, choice of analytical method and evaluation of data. For instance, in the context of imaging, these challenges encompass: (a) the selection of images magnifications being representative for all the flakes ranging in size from hundreds of nanometers to micrometers; (b) the selection of representative flakes for adequate statistics, which may involve the separation of overlapping/agglomerating flakes by segmentation; and (c) the classification of diverse morphologies such as irregularly shaped/crumpled flakes, porous flakes and particulate features present in the sample. The complexity of the analytical task has needed the introduction of specific ontology for 2D materials to identify the proper descriptors characterizing confidently the morphological features of interest. Regarding light scattering techniques such as Dynamic Light Scattering (DLS) and Multi-Angle Light Scattering (MALS) commonly used for process control in industry as a first measure, an alternative approach would be necessary. This is in part due to the use of the standard sphere-model for 2D materials as appearing to be inappropriate, whilst a disc-shape model potentially yields more suitable results. Standardization efforts are underway to establish a baseline for accurate characterization of aimed measurands with sufficient statistics. To date, the measurement methods recommended by standardization bodies for the morphological-structural characterization of GR2M’s are AFM, Raman Spectroscopy and SEM and/or TEM. The acquisition of statistically relevant numbers of flakes for a thorough characterization using TEM and AFM is particularly time-consuming. The size distribution of graphene oxide- and graphene-containing inks was investigated by using a correlative approach coupling Centrifugal Field-Flow Fractionation (CF3) [4] with MALS. Up to now, promising results for Field-Flow Fractionation have been achieved only with respect to the separation into size classes of GO samples as well as of graphene oxide mixed with graphene by Asymmetrical Field-Flow Fractionation (AF4) [5], [6]. Besides the online characterization by MALS, the eluting size fractions obtained by CF3 were also collected and subsequently measured by SEM. Successful separation into size fractions allows us to apply ensemble techniques such as MALS to samples that were previously not measurable according to best-practices. In this study, the following material sub-classes have been observed with SEM: (i) nano-graphite mixed with graphene flakes, (ii) graphene oxide few- and multi-layer flakes with diverse and highly complex morphology, and (iii) graphene oxide of well-defined size and shape with >95% single- and bilayer content were investigated. Data on the class size ranges was obtained by MALS after separation with CF3 and consideration of a disc-shape model. Significant effort was invested into the sample preparation for CF3 measurements to achieve a recovery rate of >80%, well above the recommended 70% by ISO/TS 21362:2018 for validation purposes. The material fractions collected after the CF3 measurement were separately deposited on a silicon wafer and the size results of the SEM analysis were correlated with the corresponding mean sizes obtained with MALS. T2 - Microscopy and Microanalysis 2025 CY - Salt Lake City, UTAH, USA DA - 27.07.2025 KW - Advanced Material KW - CF3 KW - SEM KW - Morphology PY - 2025 AN - OPUS4-64084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Correlative chemical imaging to reveal the nature of different commercial graphene materials N2 - Different synthesis techniques were developed which led to other graphene-related materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial. Single-layer GO flakes provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image. Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials. In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - ToF-SIMS KW - Imaging KW - Graphene-related 2D materials KW - SEM/EDX KW - Auger electron spectroscopy KW - Raman spectroscopy PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Reliable analysis of the elemental composition of graphene oxide flakes with energy dispersive spectroscopy (SEM/EDS) and x-ray photoelectron spectroscopy (XPS) N2 - Suspensions of graphene-related 2D materials (GR2M) are broadly used for further applications like printable electronics. The reliable quantification of the composition of graphene-related 2D materials as liquid suspensions is still a challenging task, which can hinder the commercialisation of the products. Specific parameters to be measured are defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present [1], but reference protocols are still missing. One of the central methods for the quantification is X-ray photoelectron spectroscopy (XPS) as a rather expensive method. Therefore, the development of cheaper alternatives is highly desired. One attractive alternative of XPS is energy-dispersive spectroscopy (EDS) which is usually coupled with scanning electron microscopy (SEM). This combination is one of the most widely used methods in analytical laboratories. In this contribution the results of a systematic study on the capability of SEM/EDS to reliably quantify the O/C ratio in a well-defined and well-characterized graphene oxide material [2] are presented. The robustness of the SEM/EDS results obtained at various measurement conditions (various excitation energies) is tested by comparing the results to the established XPS analysis [3], which has been carried out on the same samples. It is demonstrated that for samples prepared by drop-casting on a substrate, both surface-sensitive XPS analysis and bulk-characterising EDS result in very similar elemental composition of oxygen and carbon for thick spots. Further, the effect of untight deposited material enabling co-analysis of the (silicon) substrate, is evaluated for both methods, XPS and EDS. The last results clearly show the influence of the substrate on the analysis of the results and stressed out the importance of the sample preparation. T2 - E-MRS Spring Meeting CY - Strasbourg, France DA - 26.05.2025 KW - Graphene oxide KW - Reliable Analysis KW - Ionic Liquid KW - Reference Material PY - 2025 AN - OPUS4-63336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan A1 - Hörenz, Christoph T1 - Improving nanoparticle size measurement accuracy for safety assessment N2 - Nanomaterials and nanoparticles are finding applications across a wide range of technology sectors, from medicine and food to transportation and construction. In order to assess these new materials for potential risks to health and the environment, they need to be well-characterised. The measurement of constituent nanoparticle size, shape, and size distribution are important factors for the risk evaluation process. EMPIR project Improved traceability chain of nanoparticle size measurements (17NRM04, nPSize) is working to assess a range of traceable nanoparticle measurement approaches, including Scanning Electron Microscopy (also in Transmission Mode), Atomic Force Microscopy and Small Angle X-ray Scattering, and deliver improved calibration methods to users. For the techniques under investigation, physical models of their response to a range of nanoparticle types are developed. Validated reference materials will also be used for an inter-comparison of measurement systems, with an evaluation of the associated measurement uncertainty. With project contributions to standards development work, manufacturers will be better placed to assess the human and environmental risks posed by nanomaterials across a whole range of products. KW - Nanoparticles KW - Particle size distribution KW - Traceability KW - Electron microscopy KW - AFM KW - SAXS PY - 2021 UR - https://www.euramet.org/?L=0&news=40%3A1159 SP - 1 PB - EURAMET e.V. CY - Braunschweig AN - OPUS4-52129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoparticle size, shape, and concentration measurement at once – two VAMAS pre-standardization projects ready to start N2 - A case study on the TEM analysis of the size and shape distribution of TiO2 bipyramidal nanoparticles prepared on TEM grids was included in the recently published ISO standard ISO 21363. It was agreed to organize at a later stage a second inter-lab comparison with the nanoparticles distributed to the participants as a liquid suspension. Protocols for uniform nanoparticle deposition on suited supports developed and optimized within the EMPIR nPSize project are also prepared to be distributed. For this, we have chosen the VAMAS platform (www.vamas.org) which offers an excellent international infrastructure of laboratories with high competence in nanoparticle measurement. The VAMAS technical working area dedicated to nanoparticle measurement is TWA 34 ‘Nanoparticle populations’. For this type of nanoparticles, the size and shape distributions are the primary parameters to be reported. Due to the good deposition protocols developed, an automated image analysis is enabled (in contrast to the manual analysis of irregular TiO2 nanoparticles. In parallel with the TiO2 nanoparticle exercise, two spherical SiO2 nanoparticle samples with bi-modal size distributions (nominal relative number concentrations of 1:1 and 10:1) are prepared for a second VAMAS inter-lab comparison. Here, the nanoparticle concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations of the two modes. For the absolute nanoparticle concentration to be measured by imaging methods it is necessary to control the volume of the liquid suspension deposited on the substrate and to obtain such a homogeneous nanoparticle deposition on the substrate which allows to count (or extrapolate) all the deposited particles. T2 - Microscopy and Microanalysis 2021 CY - Online meeting DA - 01.08.2021 KW - Nanoparticles KW - Electron microscopy KW - VAMAS KW - Inter-laboratory comparison KW - TiO2 KW - SiO2 PY - 2021 AN - OPUS4-53065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Liaison report from VAMAS/TWA 37 Quantitative Microstructural Analysis to ISO/TC 202 Microbeam Analysis N2 - The liaison between VAMAS/TWA 37 Quantitative Microstructural Analysis and other TWAs to ISO/TC 202 Microbeam Analysis since the last Annual Meeting of ISO/TC 202 is reported. The VAMAS/TWA 37 projects initiated in the last year and the new ones in the planing phase are highlighted with technical and organisational details. Also need for more participants in 2 projects is discussed. T2 - 32nd Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - London, United Kingdom DA - 28.10.2025 KW - VAMAS KW - Quantitative microstructural analysis KW - ISO KW - Standardisation KW - Interlaboratory comparisons PY - 2025 AN - OPUS4-64552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chemello, Giovanni T1 - Characterization of Graphene using HAXPES N2 - Since its discovery, graphene has got growing attention in the industrial and application research due to its unique properties . However, graphene has not been yet implemented into the industrial market, in particularly due to the difficulty of properly characterizing this challenging material. As most of other nanomaterials, graphene’s properties are closely linked to its chemical and structural properties, such as number of layers, flake thickness, degree of functionalisation and C/O ratio. For the commercialization, suitable procedures for the measurement and characterization of the ultrathin flakes, of lateral dimensions in the range from µm to tens of µm, are essential.Surface chemical methods, especially XPS, have an outstanding role of providing chemical information on the composition. Thereby, one well-known problem for surface analytical methods is the influence of contamination on the composition as in the case of adventitious carbon. The differentiation between carbon originated from the contamination or from the graphene sample itself is often not obvious, which can lead to altered results in the determination of the composition. To overcome this problem, Hard Energy X-ray Photoelectron Spectroscopy (HAXPES) offers new possibilities due to its higher information depth. Therefore, XPS measurement obtained with Al Kα radiation (E = 1486. 6 eV) were compared with analyses performed with a Cr Kα (E = 5414. 8 eV) excitation on functionalized graphene samples. Differences are discussed in terms of potential carbon contamination, but also of oxygen on the composition of the samples. Measurements are performed on O-, N- and F-functionalized graphene. Different preparation procedures (powder, pellet, drop cast from liquid suspension) will be also discussed, correlation of the results with the flakes morphology as well as their validation with other independent methods are in progress. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Graphene KW - Functionalized graphene KW - Depth profiling PY - 2022 AN - OPUS4-56814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Chemical and structural changes at the surface of titanium materials upon irradiation with near-infrared ultrashort laser pulses N2 - Due to its large strength-to-weight ratio and excellent biocompatibility, titanium materials are of paramount importance for medical applications, e.g. as implant material for protheses. In this work, the evolution of various types of laser-induced micro- and nanostructures emerging on titanium or titanium alloys upon irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment is studied for various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz). The morphologies of the processed surfaces were systematically characterized by optical and scanning electron microscopy (OM, SEM). Complementary white-light interference microscopy (WLIM) revealed the corresponding surface topographies. Chemical and structural changes were analysed through depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray diffraction (XRD) analyses. The results point towards a remarkable influence of the laser processing parameters on the surface topography, while simultaneously altering the near-surface chemistry via laser-induced oxidation effects. Consequences for medical applications are outlined. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - ToF-SIMS KW - Chemical analysis KW - Titanium PY - 2022 AN - OPUS4-54931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Kotil, Leyla A1 - Matjacic, Lidija A1 - McMahon, Greg A1 - Bernicke, Michael A1 - Bernsmeier, Denis A1 - Kraehnert, Ralph A1 - Hertwig, Andreas A1 - Hodoroaba, Vasile-Dan T1 - Morphological and Chemical Nanoscale Analysis of Mesoporous Mixed IrOx-TiOy Thin Films as Electrode Materials N2 - orous 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 (1). 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. KW - Mesoporous thin films KW - Imaging KW - TiO2 KW - Ir oxid KW - Auger electron spectroscopy KW - ToF-SIMS KW - SEM/EDX PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.252 VL - 30 IS - Supplement 1 SP - 541 EP - 542 PB - Oxford University Press (OUP) AN - OPUS4-61185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement - What nPSize can offer to ISO/TC 229? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities, e.g. reference materials, sample preparation protocols, measurement procedures, and data analysis, to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered. The two VAMAS inter-laboratory comparisons resulted from the nSPize project and just started under TWA 34 Nanoparticle Populations (Projects #15 and #16) of bipyramidal TiO2 anatase and bimodal SiO2 nanoparticles are presented in detail. T2 - Interim Meeting of ISO/TC 229 Nanotechnologies - Strategy and Metrology Group CY - Online meeting DA - 09.05.2022 KW - Nanoparticles KW - Particle size distribution KW - Inter-laboratory comparison KW - Electron microscopy KW - AFM KW - SAXS KW - ISO/TC229 PY - 2022 AN - OPUS4-54819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Analysis of Industrial Graphene-Based Flakes – First Results on Morphological Characterization, Sample Preparation and Chemical Composition N2 - In order to bridge the gap between lab-scale and industrial-scale production of graphene it is necessary to develop processes, equipment and measurement procedures to control the material features. One of the crucial reasons of graphene’s limited commercialization is the lack of standard procedures to properly characterize and define the material chemical and structural properties down to the nanometer level. This leads to many issues regarding material synthesis repeatability, inappropriateness choice of measurands and measurement reproducibility which heavily affect the consistency of the material performance. In our study, a comparative analysis is performed on two different series (G5 and G6) of industrial graphene powders, each series produced with four types of functionalization: raw graphene, oxygen-functionalized, nitrogen-functionalized and fluorine-functionalized. All the 8 sample variants were analyzed from a chemical and morphological point of view in the form of powders prepared as slightly pressed in metallic sample holders. The results of the comparative chemical analyses XPS and EDS show a good agreement in the concentration values for all the elements present in the samples, despite the different analysis volumes addressed by the two techniques. For this reason, the samples can be considered homogeneous in both lateral and vertical direction. A clear influence of the morphology on the composition is evident. Therefore, such correlative measurements of morphology and composition are necessary for a comprehensive characterization of industrial graphene flakes. KW - Graphene powder KW - XPS KW - HAXPES KW - SEM KW - EDS KW - Functionalized graphene PY - 2022 DO - https://doi.org/10.1017/S1431927622004342 SN - 1435-8115 VL - 28 IS - Suppl 1 SP - 1006 EP - 1008 PB - Cambridge University Press CY - New York, NY AN - OPUS4-55512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - XPS of GR2M N2 - The activities of ISO-G-Scope are presented. The influence of the sample preparation and the results of XPS/HAXPES measurements are discussed. T2 - Graphene Workshop @ ISO TC 229 Meeting CY - Teddington, UK DA - 16.11.2022 KW - Graphene related materials KW - X-ray photoelectron spectroscopy KW - Sample preparation KW - Hard X-ray photoelectron spectroscopy PY - 2022 AN - OPUS4-56434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Knowledge Infrastructure supporting image-based characterisation of 2D graphene materials N2 - To better understand the relationship between image features and biological effects such as toxicity,we have developed a method combining image thresholding and pixel-wise segmentation to create annotated datasets. These datasets are used to train machine learning models and establish human–AI learning loops for material classification and structure detection. We employ deep learning architectures such as ResNet, EfficientNet, and U-Net to automate the classification and segmentation of SEM/TEM images of 2D nanomaterials, with targeted manual annotation focusing on key structures (graphene flakes, agglomerates, contaminants, etc.). This approach ensures reproducible, large-scale analysis, which is essential for studying the links between structure and biological response. Finally, our methodology aligns with OECD requirements and contributes to the Safe and Sustainable by Design (SSbD) framework, aiming to enhance product reliability and sustainability. T2 - Joint Regulatory Risk Assessors Summit – Advancing Safety & Sustainability Assessments of Advanced Materials CY - Paris, France DA - 19.06.2025 KW - Graphene KW - 2D materials KW - Knowledge infrastructure KW - Imaging KW - Machine learning PY - 2025 UR - https://macrame-project.eu/macrame-meetings-workshops/jointrras/#Agenda AN - OPUS4-63682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - How to measure the chemical composition of industrial graphene - New insights from an interlaboratory comparison N2 - International standards describing reliable protocols will facilitate the commercialization of graphene and related 2D materials. One physico-chemical key property next to flake size and thickness is the chemical composition of the material. Therefore, an ISO standard is under development with X-ray photoelectron spectroscopy having a prominent role. With its information depth of around 10 nm which is the similar length scale as the thickness as of particles of 2D materials consisting of a few monolayer XPS seems to be highly suitable for this purpose. Different sample preparation methods like pressing the powders onto adhesive tapes, into recesses, or into solid pellets result in inconsistencies in the quantification. For the validation of the quantification with XPS an interlaboratory comparison was initiated under the auspice of the “Versailles Project on Advanced Materials and Standards” (VAMAS). First results confirm that the sample preparation method (pellet vs. powder) influences the quantification results clearly. T2 - Characterization of Nanomaterials Colloquium CY - Berlin, Germany DA - 04.07.2023 KW - X-ray photoelectron spectroscopy KW - Functionalized graphene KW - Interlaboratory comparison PY - 2023 AN - OPUS4-57897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - VAMAS Regional Report Germany 2024 N2 - Regional standardisation activities and how VAMAS can help in any way to promote activities are reported. Activities related to organisational updates, government initiatives/priorities (especially related to Advanced Materials), details of any strategy documents publicly available, networks within Germany and how we engage are presented. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 49th Steering Committee Meeting CY - Rio de Janeiro, Brazil DA - 23.09.2024 KW - VAMAS KW - Advanced materials KW - Standardisation PY - 2024 UR - http://www.vamas.org/ AN - OPUS4-61405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -