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Article

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

1
Laboratoire National de Métrologie et d’Essais (LNE), 29 Avenue Roger Hennequin, CEDEX, 78197 Trappes, France
2
Dipartimento di Chimica and NIS Inter-Department Centre, University of Torino, Via P. Giuria 7, 10125 Torino, Italy
3
Academic Centre for Materials and Nanotechnology, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow, Poland
4
Federal Institute for Materials Research and Testing (BAM), Unter den Eichen 44-46, 12205 Berlin, Germany
5
Physikalisch-Technische Bundesanstalt (PTB), Abbestraße 2–12, 10587 Berlin, Germany
*
Author to whom correspondence should be addressed.
Academic Editor: David Marrero-López
Nanomaterials 2021, 11(12), 3359; https://doi.org/10.3390/nano11123359
Received: 30 September 2021 / Revised: 24 November 2021 / Accepted: 8 December 2021 / Published: 10 December 2021
(This article belongs to the Special Issue Identification and Quantification of Nanomaterials)
In this paper, the accurate determination of the size and size distribution of bipyramidal anatase nanoparticles (NPs) after deposition as single particles on a silicon substrate by correlative Scanning Electron Microscopy (SEM) with Atomic Force Microscopy (AFM) analysis is described as a new measurement procedure for metrological purposes. The knowledge of the exact orientation of the NPs is a crucial step in extracting the real 3D dimensions of the particles. Two approaches are proposed to determine the geometrical orientation of individual nano-bipyramides: (i) AFM profiling along the long bipyramid axis and (ii) stage tilting followed by SEM imaging. Furthermore, a recently developed method, Transmission Kikuchi Diffraction (TKD), which needs preparation of the crystalline NPs on electron-transparent substrates such as TEM grids, has been tested with respect to its capability of identifying the geometrical orientation of the individual NPs. With the NPs prepared homogeneously on a TEM grid, the transmission mode in a SEM, i.e., STEM-in-SEM (or T-SEM), can be also applied to extract accurate projection dimensions of the nanoparticles from the same sample area as that analysed by SEM, TKD and possibly AFM. Finally, Small Angle X-ray Scattering (SAXS) can be used as an ensemble technique able to measure the NPs in liquid suspension and, with ab-initio knowledge of the NP shape from the descriptive imaging techniques, to provide traceable NP size distribution and particle concentration. View Full-Text
Keywords: nanoparticle; complex-shape; bipyramid; electron microscopy; atomic force microscopy; size measurements; TKD; STEM-in-SEM; SAXS; nanoparticle concentration; correlative analysis nanoparticle; complex-shape; bipyramid; electron microscopy; atomic force microscopy; size measurements; TKD; STEM-in-SEM; SAXS; nanoparticle concentration; correlative analysis
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MDPI and ACS Style

Crouzier, L.; Feltin, N.; Delvallée, A.; Pellegrino, F.; Maurino, V.; Cios, G.; Tokarski, T.; Salzmann, C.; Deumer, J.; Gollwitzer, C.; Hodoroaba, V.-D. Correlative Analysis of the Dimensional Properties of Bipyramidal Titania Nanoparticles by Complementing Electron Microscopy with Other Methods. Nanomaterials 2021, 11, 3359. https://doi.org/10.3390/nano11123359

AMA Style

Crouzier L, Feltin N, Delvallée A, Pellegrino F, Maurino V, Cios G, Tokarski T, Salzmann C, Deumer J, Gollwitzer C, Hodoroaba V-D. Correlative Analysis of the Dimensional Properties of Bipyramidal Titania Nanoparticles by Complementing Electron Microscopy with Other Methods. Nanomaterials. 2021; 11(12):3359. https://doi.org/10.3390/nano11123359

Chicago/Turabian Style

Crouzier, Loïc, Nicolas Feltin, Alexandra Delvallée, Francesco Pellegrino, Valter Maurino, Grzegorz Cios, Tomasz Tokarski, Christoph Salzmann, Jérôme Deumer, Christian Gollwitzer, and Vasile-Dan Hodoroaba. 2021. "Correlative Analysis of the Dimensional Properties of Bipyramidal Titania Nanoparticles by Complementing Electron Microscopy with Other Methods" Nanomaterials 11, no. 12: 3359. https://doi.org/10.3390/nano11123359

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