Nanomaterials (Mar 2023)

Metrological Protocols for Reaching Reliable and SI-Traceable Size Results for Multi-Modal and Complexly Shaped Reference Nanoparticles

  • Nicolas Feltin,
  • Loïc Crouzier,
  • Alexandra Delvallée,
  • Francesco Pellegrino,
  • Valter Maurino,
  • Dorota Bartczak,
  • Heidi Goenaga-Infante,
  • Olivier Taché,
  • Sylvie Marguet,
  • Fabienne Testard,
  • Sébastien Artous,
  • François Saint-Antonin,
  • Christoph Salzmann,
  • Jérôme Deumer,
  • Christian Gollwitzer,
  • Richard Koops,
  • Noham Sebaïhi,
  • Richard Fontanges,
  • Matthias Neuwirth,
  • Detlef Bergmann,
  • Dorothee Hüser,
  • Tobias Klein,
  • Vasile-Dan Hodoroaba

DOI
https://doi.org/10.3390/nano13060993
Journal volume & issue
Vol. 13, no. 6
p. 993

Abstract

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The study described in this paper was conducted in the framework of the European nPSize project (EMPIR program) with the main objective of proposing new reference certified nanomaterials for the market in order to improve the reliability and traceability of nanoparticle size measurements. For this purpose, bimodal populations as well as complexly shaped nanoparticles (bipyramids, cubes, and rods) were synthesized. An inter-laboratory comparison was organized for comparing the size measurements of the selected nanoparticle samples performed with electron microscopy (TEM, SEM, and TSEM), scanning probe microscopy (AFM), or small-angle X-ray scattering (SAXS). The results demonstrate good consistency of the measured size by the different techniques in cases where special care was taken for sample preparation, instrument calibration, and the clear definition of the measurand. For each characterization method, the calibration process is described and a semi-quantitative table grouping the main error sources is proposed for estimating the uncertainties associated with the measurements. Regarding microscopy-based techniques applied to complexly shaped nanoparticles, data dispersion can be observed when the size measurements are affected by the orientation of the nanoparticles on the substrate. For the most complex materials, hybrid approaches combining several complementary techniques were tested, with the outcome being that the reliability of the size results was improved.

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