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52. Elemental composition and thickness determination of thin films by electron probe microanalysis.

Author

Terborg, Ralf, Kim, Kyung Joong, and Hodoroaba, Vasile‐Dan

Subjects
ELECTRON probe microanalysis, THIN films, INDUCTIVELY coupled plasma mass spectrometry, GERMANIUM films
Abstract

Electron probe microanalysis (EPMA) applies to solid samples of homogenous (bulk) chemical composition and can usually not be applied to structures which are inhomogeneous in the micrometer range such as thin film systems down to a few nm. However, in combination with the established thin film software Stratagem, the thickness as well as the elemental composition of thin films on a substrate can be determined. This has been recently successfully demonstrated for Fe‐Ni on Si and Si‐Ge on Al2O3 thin film systems. For both systems five samples of different elemental composition and a reference were produced and characterised by inductively coupled plasma mass spectrometry (ICP‐MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM) as reference values. Last year, a new and open‐source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k‐ratios). In this contribution, we re‐evaluated the data acquired for the Fe‐Ni and Si‐Ge systems using the BadgerFilm software package and compared the obtained elemental compositions and thickness values with the results of the Stratagem software and the reference methods. The conclusion is that the BadgerFilm software shows good agreement with the elemental composition and thickness calculated by Stratagem (mostly <2% for both composition and thickness) and with the reference values for two representative thin film systems (<1%–2% for composition and <10%–20% for thickness). [ABSTRACT FROM AUTHOR]

Published
2023
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61. Correction: Peters et al. Benchmarking the ACEnano Toolbox for Characterisation of Nanoparticle Size and Concentration by Interlaboratory Comparison. Molecules 2021, 26, 5315

Author

Peters, Ruud, primary, Elbers, Ingrid, additional, Undas, Anna, additional, Sijtsma, Eelco, additional, Briffa, Sophie, additional, Carnell-Morris, Pauline, additional, Siupa, Agnieszka, additional, Yoon, Tae-Hyun, additional, Burr, Loïc, additional, Schmid, David, additional, Tentschert, Jutta, additional, Hachenberger, Yves, additional, Jungnickel, Harald, additional, Luch, Andreas, additional, Meier, Florian, additional, Kocic, Jovana, additional, Kim, Jaeseok, additional, Park, Byong Chon, additional, Hardy, Barry, additional, Johnston, Colin, additional, Jurkschat, Kerstin, additional, Radnik, Jörg, additional, Hodoroaba, Vasile-Dan, additional, Lynch, Iseult, additional, and Valsami-Jones, Eugenia, additional

Published
2022
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64. Correction : Benchmarking the ACEnano Toolbox for Characterisation of Nanoparticle Size and Concentration by Interlaboratory Comparison (Molecules, (2021), 26, (5315), 10.3390/molecules26175315)

Author

Peters, Ruud, Elbers, Ingrid, Undas, Anna, Sijtsma, Eelco, Briffa, Sophie, Carnell-Morris, Pauline, Siupa, Agnieszka, Yoon, Tae Hyun, Burr, Loïc, Schmid, David, Tentschert, Jutta, Hachenberger, Yves, Jungnickel, Harald, Luch, Andreas, Meier, Florian, Kocic, Jovana, Kim, Jaeseok, Park, Byong Chon, Hardy, Barry, Johnston, Colin, Jurkschat, Kerstin, Radnik, Jörg, Hodoroaba, Vasile Dan, Lynch, Iseult, Valsami-Jones, Eugenia, Peters, Ruud, Elbers, Ingrid, Undas, Anna, Sijtsma, Eelco, Briffa, Sophie, Carnell-Morris, Pauline, Siupa, Agnieszka, Yoon, Tae Hyun, Burr, Loïc, Schmid, David, Tentschert, Jutta, Hachenberger, Yves, Jungnickel, Harald, Luch, Andreas, Meier, Florian, Kocic, Jovana, Kim, Jaeseok, Park, Byong Chon, Hardy, Barry, Johnston, Colin, Jurkschat, Kerstin, Radnik, Jörg, Hodoroaba, Vasile Dan, Lynch, Iseult, and Valsami-Jones, Eugenia

Abstract

Due to miscommunication a number of potential co-authors were not listed in the original publication [1]. The actual list of authors should be as follows All co-authors agree with the content of this correction and wish to apologize for any inconvenience to the readers resulting from this error

Published
2022

66. Report on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis and by machine learning (Deliverable D5)

Author

Fontanges, Richard, Hodoroaba, Vasile-Dan, Crouzier, Loïc, Feltin, Nicolas, Delvallée, Alexandra, Deumer, Jérôme, Gollwitzer, Christian, Klein, Tobias, Salzmann, Christoph, Koops, Richard, Sebaïhi, Noham, Pauw, Brian R., Smales, Glen, Artous, Sébastien, and Taché, Olivier

Subjects
size measurement, physical basis, machine learning, nanoparticle detection, algorithm sequences
Abstract

The main objective of the nPSize project is to improve the measurement capabilities for nanoparticle size based on both measurement methods traceable to SI units and new reference materials. Two basic approaches have been used in order to develop measurement procedures resulting in traceable results of the nanoparticle size distribution: physical modelling for the methods used in the project (TSEM, SEM, AFM and SAXS) and machine learning. Physical modelling:In this part, the physical models associated with different shape measurements for the techniques TSEM, SEM, AFM and SAXS have been collected and further developed with the aim to simulate the resulting signal as measured by the individual methods. Uncertainties and traceability associated with each model were investigated and evaluated. In the following, the progress on these physical models is reported for each individual method. Machine Learning modelling:The aim of this part is to use machine learning to enable automatic measurement of nanoparticle shape from expert a-priori information only. No physical model will be used as a-priori information in this task. The accuracy and traceability of the size results obtained by each technique will be analyzed and compared with the physical modelling. A machine learning database will then be used to create automatic detection algorithms.

Published
2021
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67. Automation and Standardization—A Coupled Approach Towards Reproducible Sample Preparation Protocols for Nanomaterial Analysis

Author

Radnik, Jörg, primary, Hodoroaba, Vasile-Dan, additional, Jungnickel, Harald, additional, Tentschert, Jutta, additional, Luch, Andreas, additional, Sogne, Vanessa, additional, Meier, Florian, additional, Burr, Loïc, additional, Schmid, David, additional, Schlager, Christoph, additional, Yoon, Tae Hyun, additional, Peters, Ruud, additional, Briffa, Sophie M., additional, and Valsami-Jones, Eugenia, additional

Published
2022
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70. Correlative Analysis of the Dimensional Properties of Bipyramidal Titania Nanoparticles by Complementing Electron Microscopy with Other Methods

Author

Crouzier, Loïc, primary, Feltin, Nicolas, additional, Delvallée, Alexandra, additional, Pellegrino, Francesco, additional, Maurino, Valter, additional, Cios, Grzegorz, additional, Tokarski, Tomasz, additional, Salzmann, Christoph, additional, Deumer, Jérôme, additional, Gollwitzer, Christian, additional, and Hodoroaba, Vasile-Dan, additional

Published
2021
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74. Benchmarking the ACEnano Toolbox for Characterisation of Nanoparticle Size and Concentration by Interlaboratory Comparisons

Author

Peters, Ruud, primary, Elbers, Ingrid, additional, Undas, Anna, additional, Sijtsma, Eelco, additional, Briffa, Sophie, additional, Carnell-Morris, Pauline, additional, Siupa, Agnieszka, additional, Yoon, Tae-Hyun, additional, Burr, Loïc, additional, Schmid, David, additional, Tentschert, Jutta, additional, Hachenberger, Yves, additional, Jungnickel, Harald, additional, Luch, Andreas, additional, Meier, Florian, additional, Kocic, Jovana, additional, Kim, Jaeseok, additional, Park, Byong, additional, Hardy, Barry, additional, Johnston, Colin, additional, Jurkschat, Kerstin, additional, Radnik, Jörg, additional, Hodoroaba, Vasile-Dan, additional, Lynch, Iseult, additional, and Valsami-Jones, Eugenia, additional

Published
2021
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82. Efficient Luminescent Solar Concentrators Based on Environmentally Friendly Cd‐Free Ternary AIS/ZnS Quantum Dots

Author

Dhamo, Lorena, Carulli, Francesco, Nickl, Philip, Wegner, Karl David, Hodoroaba, Vasile-Dan, Würth, Christian, Brovelli, Sergio, Resch-Genger, Ute, Dhamo, Lorena, Carulli, Francesco, Nickl, Philip, Wegner, Karl David, Hodoroaba, Vasile-Dan, Würth, Christian, Brovelli, Sergio, and Resch-Genger, Ute

Abstract

Luminescent solar concentrators (LSC) allow to obtain renewable energy from building integrated photovoltaic systems. As promising efficient and long-term stable LSC fluorophores semiconductor nanocrystals like quantum dots (QDs) with size and composition tunable optoelectronic properties have recently emerged. The most popular II/VI or IV/VI semiconductor QDs contain, however, potentially hazardous cadmium or lead ions, which is a bottleneck for commercial applications. A simple aqueous based, microwave-assisted synthesis for environmentally friendly and highly emissive AgInS2/ZnS QDs is developed using 3-mercaptopropionic acid (MPA) and glutathione (GSH) and their incorporation into polylaurylmethacrylate (PLMA) polymer slabs integrable in LSC devices (10.4 × 10.4 × 0.2 cm3, G = 12.98). With this simple approach, optical power efficiencies (OPE) of 3.8% and 3.6% and optical quantum efficiencies (OQE) of 24.1% and 27.4% are obtained, which are among the highest values yet reported., German Research Council, European Union's Horizon 2020, Marie Sklodowska‐Curie, Deutsche Forschungsgemeinschaft http://dx.doi.org/10.13039/501100001659, Peer Reviewed

Published
2021

83. Efficient Luminescent Solar Concentrators Based on Environmentally Friendly Cd‐Free Ternary AIS/ZnS Quantum Dots

Author

Dhamo, L, Carulli, F, Nickl, P, Wegner, K, Hodoroaba, V, Würth, C, Brovelli, S, Resch‐genger, U, Dhamo, Lorena, Carulli, Francesco, Nickl, Philip, Wegner, Karl David, Hodoroaba, Vasile‐Dan, Würth, Christian, Brovelli, Sergio, Resch‐Genger, Ute, Dhamo, L, Carulli, F, Nickl, P, Wegner, K, Hodoroaba, V, Würth, C, Brovelli, S, Resch‐genger, U, Dhamo, Lorena, Carulli, Francesco, Nickl, Philip, Wegner, Karl David, Hodoroaba, Vasile‐Dan, Würth, Christian, Brovelli, Sergio, and Resch‐Genger, Ute

Abstract

Luminescent solar concentrators (LSC) allow to obtain renewable energy from building integrated photovoltaic systems. As promising efficient and long-term stable LSC fluorophores semiconductor nanocrystals like quantum dots (QDs) with size and composition tunable optoelectronic properties have recently emerged. The most popular II/VI or IV/VI semiconductor QDs contain, however, potentially hazardous cadmium or lead ions, which is a bottleneck for commercial applications. A simple aqueous based, microwave-assisted synthesis for environmentally friendly and highly emissive AgInS2/ZnS QDs is developed using 3-mercaptopropionic acid (MPA) and glutathione (GSH) and their incorporation into polylaurylmethacrylate (PLMA) polymer slabs integrable in LSC devices (10.4 × 10.4 × 0.2 cm3, G = 12.98). With this simple approach, optical power efficiencies (OPE) of 3.8% and 3.6% and optical quantum efficiencies (OQE) of 24.1% and 27.4% are obtained, which are among the highest values yet reported.

Published
2021

84. Benchmarking the acenano toolbox for characterisation of nanoparticle size and concentration by interlaboratory comparisons

Author

Peters, Ruud, Elbers, Ingrid, Undas, Anna, Sijtsma, Eelco, Briffa, Sophie, Carnell-Morris, Pauline, Siupa, Agnieszka, Yoon, Tae Hyun, Burr, Loïc, Schmid, David, Tentschert, Jutta, Hachenberger, Yves, Jungnickel, Harald, Luch, Andreas, Meier, Florian, Radnik, Jörg, Hodoroaba, Vasile Dan, Lynch, Iseult, Valsami-Jones, Eugenia, Peters, Ruud, Elbers, Ingrid, Undas, Anna, Sijtsma, Eelco, Briffa, Sophie, Carnell-Morris, Pauline, Siupa, Agnieszka, Yoon, Tae Hyun, Burr, Loïc, Schmid, David, Tentschert, Jutta, Hachenberger, Yves, Jungnickel, Harald, Luch, Andreas, Meier, Florian, Radnik, Jörg, Hodoroaba, Vasile Dan, Lynch, Iseult, and Valsami-Jones, Eugenia

Abstract

ACEnano is an EU-funded project which aims at developing, optimising and validating methods for the detection and characterisation of nanomaterials (NMs) in increasingly complex matrices to improve confidence in the results and support their use in regulation. Within this project, several interlaboratory comparisons (ILCs) for the determination of particle size and concentration have been organised to benchmark existing analytical methods. In this paper the results of a number of these ILCs for the characterisation of NMs are presented and discussed. The results of the analyses of pristine well-defined particles such as 60 nm Au NMs in a simple aqueous suspension showed that laboratories are well capable of determining the sizes of these particles. The analysis of particles in complex matrices or formulations such as consumer products resulted in larger variations in particle sizes within technologies and clear differences in capability between techniques. Sunscreen lotion sample analysis by laboratories using spICP-MS and TEM/SEM identified and confirmed the TiO2 particles as being nanoscale and compliant with the EU definition of an NM for regulatory purposes. In a toothpaste sample orthogonal results by PTA, spICP-MS and TEM/SEM agreed and stated the TiO2 particles as not fitting the EU definition of an NM. In general, from the results of these ILCs we conclude that laboratories are well capable of determining particle sizes of NM, even in fairly complex formulations.

Published
2021

95. Customizing New Titanium Dioxide Nanoparticles with Controlled Particle Size and Shape Distribution: A Feasibility Study Toward Reference Materials for Quality Assurance of Nonspherical Nanoparticle Characterization.

Author

Pellegrino, Francesco, Ortel, Erik, Mielke, Johannes, Schmidt, Roland, Maurino, Valter, and Hodoroaba, Vasile-Dan

Subjects
TITANIUM dioxide nanoparticles, PARTICLE size distribution, REFERENCE sources, QUALITY assurance, FEASIBILITY studies
Abstract

An overview is given on the synthesis of TiO2 nanoparticles with well‐defined nonspherical shapes (platelet like, bipyramidal, and elongated), with the focus on controlled, reproducible synthesis, as a key requirement for the production of reference materials with homogeneous and stable properties. Particularly with regard to the nanoparticle shapes, there is a high need of certified materials, solely one material of this type being commercially available since a few months (elongated TiO2). Further, measurement approaches with electron microscopy as the golden method to tackle the nanoparticle shape are developed to determine accurately the size and shape distribution for such nonspherical particles. A prerequisite for accurate and easy (i.e., automated) image analysis is the sample preparation, which ideally must ensure a deposition of the nanoparticles from liquid suspension onto a substrate such that the particles do not overlap, are solvent‐free, and have a high deposition density. Challenges in the synthesis of perfectly monodispersed and solvent‐free TiO2 nanoparticles of platelet and acicular shapes are highlighted as well as successful measurement approaches on how to extract from 2D projection electron micrographs the most accurate spatial information, that is, true 3D size, for example, of the bipyramidal nanoparticles with different geometrical orientations on a substrate. [ABSTRACT FROM AUTHOR]

Published
2022
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96. Ellipsometry‐Based Approach for the Characterization of Mesoporous Thin Films for H2 Technologies.

Author

Sachse, René, Moor, Maëlle, Kraehnert, Ralph, Hodoroaba, Vasile-Dan, and Hertwig, Andreas

Subjects
THIN films, ELLIPSOMETRY, ELECTRONIC structure, ELECTRONIC materials, REFERENCE sources, CHEMICAL processes
Abstract

Porous thin layer materials are gaining importance in different fields of technology and pose a challenge to the accurate determination of materials' properties important for their function. Herein, a hybrid measurement technique using ellipsometry together with other independent methods for validation, is demonstrated. Ellipsometry provides information about the porosity of different mesoporous films (PtRuNP/OMC = 45%; IrOx = 46%) as well as about the pore size (pore radius of ≈5 nm for PtRuNP/OMC). In addition, the electronic structure of a material, such as intraband transitions of a mesoporous IrOx film, can be identified, which can be used to better understand the mechanisms of chemical processes. In addition, it is shown that ellipsometry can be used as a scalable imaging and visualization method for quality assurance in production. These require accurate and traceable measurements, with reference materials playing an important role that include porosity and other related properties. It is shown that novel analytical methods are useful for improving analytical work in this entire field. [ABSTRACT FROM AUTHOR]

Published
2022
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97. Cover Image, Volume 138, Issue 12

Author

Cano Murillo, Natalia, primary, Ghasem Zadeh Khorasani, Media, additional, Silbernagl, Dorothee, additional, Hahn, Marc Benjamin, additional, Hodoroaba, Vasile‐Dan, additional, and Sturm, Heinz, additional

Published
2020
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99. Assessing Optical and Electrical Properties of Highly Active IrOx Catalysts for the Electrochemical Oxygen Evolution Reaction via Spectroscopic Ellipsometry

Author

Sachse, René, primary, Pflüger, Mika, additional, Velasco-Vélez, Juan-Jesús, additional, Sahre, Mario, additional, Radnik, Jörg, additional, Bernicke, Michael, additional, Bernsmeier, Denis, additional, Hodoroaba, Vasile-Dan, additional, Krumrey, Michael, additional, Strasser, Peter, additional, Kraehnert, Ralph, additional, and Hertwig, Andreas, additional

Published
2020
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