More than ever before, materials-driven product innovations in industry and shorter time-to-market introductions for new products require high advancement rates and a tight coupling between research, development and manufacturing. Analytical techniques and respective tools, particularly to investigate nanomaterials, are considered to be fundamental drivers for innovation in industry.
As a consequence, this symposium will cover data acquisition and data analysis of nano-scale materials along the whole value and innovation chain, from fundamental research up to industrial applications. It will bring materials scientists and computer scientists together from universities, research institutions, equipment manufacturers and industrial end-users. New results from the combined utilization of analytical techniques will be reported in several talks and in the poster sessions, and novel solutions in the field of materials characterization and data analysis for process and quality control will be shown. The discussions and interactions between the stakeholders will help to identify gaps in the fields of correlative materials characterization and to propose actions to close them and to support industrial exploitation of innovative materials. The symposium aims at reinforcing ongoing collaborations and discussing ideas for new collaborations.
Resume : I will show how an in-depth description of the basic principles of diffraction-unlimited fluorescence microscopy (nanoscopy) [1] has spawned a new powerful superresolution concept, namely MINFLUX nanoscopy [2-5]. MINFLUX utilizes a local excitation intensity minimum (of a doughnut or a standing wave) that is targeted like a probe in order to localize the fluorescent molecule to be registered. In combination with single-molecule switching, MINFLUX and its more recent ?cousin? MINSTED [6] have obtained the ultimate (super)resolution: the size of a molecule. Providing 1?3 nanometer resolution these novel microscopy concepts are being established for routine fluorescence imaging at the highest, molecular-size resolution levels. Relying on fewer detected photons than popular camera-based localization, MINFLUX and MINSTED nanoscopy are poised to open a new chapter in the imaging of protein complexes and distributions in fixed and living cells.[1]Hell, S.W. Nat. Methods 6, 24-32 (2009). [2] Balzarotti, F., Eilers, Y., Gwosch, K. C., Gynn, A. H., Westphal, V., Stefani, F. D., Elf, J., Hell, S.W. Science 355, 606-612 (2017). [3]Eilers, Y., Ta, H., Gwosch, K. C., Balzarotti, F., Hell, S. W. PNAS 115, 6117-6122 (2018).[4]Gwosch, K. C., Pape, J. K., Balzarotti, F., Hoess, P., Ellenberg, J., Ries, J., Hell, S. W. Nat. Methods 17, 217-224 (2020)[5]Schmidt R., Weihs T., Wurm C., Janssen I., Rehman J., Sahl S.J., Hell S.W. Nat Commun 12:1478 (2021)[6]Weber, M., Leutenegger M., Stoldt S., Jakobs S., Mihaila T.S., Butkevitch A.N., Hell S.W., Nat. Photonics, -021-00774-2 (2021).
Resume : Metal clusters supported on zeolites (metal@zeolite) are attractive due to their catalytic activity combined with zeolite shape selectivity [1]. Various synthetic strategies are used for rational preparation of metal@zeolite composites. The main goal of this study is to stabilize metal species and precisely control their size and distribution [2]. The understanding of the synthesis mechanisms and metal-zeolite interactions is still insufficient, thus the experimental and theoretical research of these materials is required [3]. Recently, we reported a series of metal@zeolite materials prepared using the 4-step ADOR (assembly-disassembly-organization-reassembly) strategy [4]. ADOR approach is based on topotactic transformation of UTL germanosilicate to layered precursor followed by organization of layers and reassembly of them generating a set of isoreticular zeolites (IPC family of materials). Utilization of this method allowed preparation of zeolites with various porosity with incorporated metal nanoparticles i.e. Pt@IPC-2 (OKO), Pt@IPC-4 (PCR) [4] and others. This set of materials consists of the same layers with different connectivity, which make them a suitable model to explore the dynamic structural evolution of metal clusters.Herein, we report the incorporation of rhodium species into ADOR zeolites. We investigated the dynamic structural change of Rh clusters and their thermal stability by performing in-situ heating of the material in scanning transmission electron microscope (STEM). Using a heating holder, we performed a step-wise temperature treatment (from the room temperature up to 700 oC) and analyzed changes in size of metal nanoparticles by STEM imaging. Moreover, properties of samples were investigated by PXRD, sorption of Ar, SEM, and EDS. Catalytic performance of prepared materials was tested in hydrogenation of nitriles. Chemical properties and architecture of the of zeolite support play a significant role in the formation and stability of Rh nanoparticles.References1.Liu, L. C., Corma, A., Nature Reviews Materials (2020) 1-202.Wang, H., Wang, L., Xiao, F. S., ACS Central Science 6 (2020) 1685-1697.3.Liu, L. C., Zakharov, D. N., Arenal, R., Concepcion, P., Stach, E. A., Corma, A., Nature communications 9 (2018) 574.4.Zhang, Y. Y., Kubu, M., Mazur, M., Cejka, J., Microporous and Mesoporous Materials 279 (2019) 364-370.
Resume : Correlating HR-TEM and XPS to elucidate the core-shell structure of ultrabright CdSE/CdS semiconductor quantum dotsJrg Radnik(1), Florian Weigert (2), Ines Husler (3), Daniel Geiler (2), and Ute Resch-Genger(2)1 Federal Institute for Material Research and Testing (BAM), Division 6.1 Surface Analysis and Interfacial Chemistry, Unter den Eichen 44-46, 12203 Berlin Germany;2 Federal Institute for Material Research and Testing (BAM), Division 1.2 Biophotonics, Richard-Willsttter-Str. 11, 12489 Berlin Germany3 Technische Universitt Berlin, Institut fr Optik und Atomare Physik, Strae des 17. Juni 135, 10623 Berlin, GermanyControlling the thickness and tightness of surface passivation shells is crucial for many applications of core-shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the application-relevant functionality like a high photoluminescence (PL) quantum yield. This calls for a whole nanoobject approach. Moreover, the thickness of the organic coating remains often unclear.By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. The results of the different methods match very well within the different measurement uncertainties. Additionally, results obtained with energy-resolved XPS using excitation energies between 200 eV and 800 eV are discussed with respect to a potential core/shell intermixing. Moreover, the future application potential of this approach correlating different sizing and structural methods is discussed considering the method-inherent uncertainties and other core/multi-shell nanostructures. The authors gratefully acknowledge financial support from the German Research Foundation (DFG grant RE1203/12-3) and from the European Metrology Programme for Innovation and Research (EMPIR) as part of the project 14IND12 INNANOPART.
Resume : To enable the development of technology fields, such as artificial intelligence and big data, integrated circuits, also called microchips, have to meet new performance requirements. This can be achieved by scaling down the transistor size and increasing the density of the device. This area scaling in the front-end of line (FEoL) is connected with an even accelerated size reduction in the back-end of line (BEOL), the so called interconnects, and leads to smaller metal pitches and reduced cross-sectional areas of the wires. But this size reduction to the smaller nanometer range is connected with many material challenges, due to an increasing resistance-capacitance (RC) delay.In order to reduce the resistance of the interconnects, novel diffusion barriers with a lower resistivity are integrated and the thickness of them is reduced to a minimum. Additionally the standard interconnect material copper is replaced by other metals, such as ruthenium or cobalt. Although those metals have a higher bulk resistivity than copper, due to their shorter electron mean free path, a resistance reduction can be achieved in small features with critical dimensions below 15 nm [1]. To maintain the functionality and reliability of the device it is therefore necessary to understand the diffusion mechanism at the interfaces of the new integrated materials.In our work we used X-ray photoelectron spectroscopy depth profiling (XPS-DP) to describe the diffusion of interconnect metals into novel barrier materials, consisting of different metal alloys. Diffusion was induced by annealing of the material stacks at different temperatures in a rapid thermal annealing system. Following we applied the Mixing-Roughness-Information Depth (MRI) model, which was developed by Hofmann et al. [2], to estimate the diffusion coefficients from the XPS depth profiles. The MRI model describes the depth resolution function (DRF) of the sputter profiles and hence can account for the sputter-induced broadening of the depth profile. The model is based on three physical well defined parameters, atomic mixing (w), information depth (?) and roughness (?), that are described by 3 different functions. The convolution of those functions will give the DRF. Following the roughness parameter (?) can be used to quantify the diffusion as it is directly correlated to the diffusion by the relation: ?2= 2Dt [2]. Hence by applying the model to the XPS depth profiles of the as-deposited thin film stacks as well as to the annealed stacks, diffusion coefficients can be estimated and the diffusion behavior at the interface of those novel materials can be directly compared. Additionally to the just described simple MRI model, an extended version was used to account for preferential sputtering in some of the thin films stacks. Here the concentration depth profile will be corrected by the different sputter rates of the materials by applying a differential equation that describes the surface concentration in the mixing zones [3].In summary we show that this analysis method is suitable to quantify the diffusion in different thin film stacks and that it can be used to describe the diffusion mechanisms in interconnects in more detail.[1] M. Naik, ?Interconnect Trend for Single Digit Nodes?, IEDM 2018[2] S. Hofmann, Auger- and X-Ray Photoelectron Spectroscopy in Materials Science, Springer, 2013, p. 349-350[3] S. Hofmann et al., 2019, Preferential sputtering effects in depth profiling of multilayers with SIMS, XPS and AES, Applied Surface Science 483, p. 140?155.