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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.
We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds, and the segmented images can be used for automatically extracting and calculating various other particle size and shape descriptors.
The Competence Centre nano@BAM is presenting a new X-ray Photoelectron Spectrometer – the HAXPES (XPS at hard energy) – for researching advanced materials at the nanoscale. With HAXPES detailed chemical information can now be gained not only from the first outermost nanometres of the sample surface, but also from deeper regions.
Top international experts will share their knowledge and key findings on how to utilise HAXPES for exploring the surface of various advanced materials. Following the lectures, we will show you a short demo of the new instrument and answer your questions.
One of the objectives of the EU Project EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials & Nanotechnologies) was to test and benchmark the services in order to check their relevance to address identified stakeholder needs, but also to evaluate the governance of the structure delivering the proposed services. The aim is to demonstrate the technical relevance of the services and the overall open structure organisation, including governance rules and operating procedures, by answering relevant identified questions (case studies) selected by a panel of stakeholders. Therefore, a significant part of the project will be devoted to this demonstration of the operational and functional basis of the organized network.
This presentation is structured in two parts: i) Hybrid metrology by combining SEM with AFM (N. Feltin) and ii) hybridization and corelative microscopy by SEM, STEM-in-SEM, TEM, EDS, Auger Electron Microscopy, TKD and more (D. Hodoroaba).
The first part is focused on the metrological part of the hybrid measurement SEM-AFM, the second part offers some further possibilities of correlative microscopy of nanoparticles based on practical examples.
Nanoparticle Populations
(2022)
Two new projects P15 Measurement of particle size and shape distribution of bipyramidal titania including deposition from liquid suspension and P16 Measurement of (relative) number concentration of bimodal silica nanoparticles including deposition from liquid suspension have been started at VAMAS/TWA 34 under the lead of BAM. First results are presented and discussed.
Quantitative Microstructural Analysis - VAMAS TWA 37 & Liaison with ISO/TC 202 Microbeam Analysis
(2022)
The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. The recently started project FIB sample processing for TEM is highlighted. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. Further, a short overview of the VAMAS areas of activities is given where Germany is involved. Planed regional VAMAS Workshops in Germany in 2023 are announced.
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.
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.
Experience gained at BAM within the European project ISGScope on the accurate measureemnt of graphene oxide flakes by electron microscopy is presented. Particularly, factors such as the type of solvent, substrate temperature, but also proper, gentle measurement parameters and image analysis conditions towards automation are highlighted. The measurement procedures in develeopment are being prepared to launch an inter-laboratory comparison under VAMAS (TWA41) as preparatory guidance for future standardisation at ISO.