Dimensional metrology at the nanoscale: quantitative characterization of nanoparticles by means of metrological atomic force microscopy

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INRiM Technical Report 26/2020 - Indoor and outdoor measurements of particulate matter concentration in air during wintertime performed in INRiM Campus and in the CNR Research Area of Turin by using particle counters

This technical report shows the study of the concentration of particulate matter in air performed in different environments (outdoor, indoor and in underground laboratories) by using two particle counters. Measurements were carried out in different climatic conditions during wintertime over three weeks into INRiM Campus and in the CNR Research Area of Turin. In order to compare the results obtained using portable airborne particle counter with those of A.R.P.A. Piemonte, a spreadsheet for transforming particles number in air into particles concentration was implemented, by assuming a spherical shape of the particles and a density d = 1 g ∙ cm−3. Finally, two different particle analysers are compared, obtaining a result agreement within 13 %

AFM Measurements and Tip Characterization of Nanoparticles with Different Shapes

Unambiguous identification of the measurement methodologies is fundamental to reduce the uncertainty and support traceability of particle shape and size at the nanoscale. In this work, the critical aspects in atomic force microscopy measurements, that is, drawbacks on sample preparation, instrumental parameters, image pre-processing, size reconstruction, and tip enlargement, are discussed in reference to quantitative dimensional measurements on different kinds of nanoparticles (inorganic and biological) with different shapes (spherical, cylindrical, complex geometry). Once the cross-section profile is extracted, top-height measurements on isolated nanoparticles of any shape can be achieved with sub-nanometer accuracy. Lateral resolution is affected by the pixel size and shape of the probe, causing dilation in the atomic force microscopy image. For the reconstruction of critical sizes of inorganic non-spherical nanoparticles, a geometric approach that considers the nominal shape because of the synthesis conditions is presented and discussed

AFM Measurements and Tip Characterization of Nanoparticles with Different Shapes

Unambiguous identification of the measurement methodologies is fundamental to reduce the uncertainty and support traceability of particle shape and size at the nanoscale. In this work, the critical aspects in atomic force microscopy measurements, that is, drawbacks on sample preparation, instrumental parameters, image pre-processing, size reconstruction, and tip enlargement, are discussed in reference to quantitative dimensional measurements on different kinds of nanoparticles (inorganic and biological) with different shapes (spherical, cylindrical, complex geometry). Once the cross-section profile is extracted, top-height measurements on isolated nanoparticles of any shape can be achieved with sub-nanometer accuracy. Lateral resolution is affected by the pixel size and shape of the probe, causing dilation in the atomic force microscopy image. For the reconstruction of critical sizes of inorganic non-spherical nanoparticles, a geometric approach that considers the nominal shape because of the synthesis conditions is presented and discussed

Quantitative three-dimensional characterization of critical sizes of non-spherical TiO2 nanoparticles by using atomic force microscopy

Since both size and shape of nanoparticles are challenging to be quantitatively measured, traceable 3D measurements are nowadays an issue. 3D nanometrology plays a crucial role to reduce the uncertainty of measurements, improve traceable calibration of samples and implement new approaches, models, and methodologies in the study of the nanomaterials. AFM measurement of nanoparticles with unusual shape represent a non-trivial challenge due to the convolution with the finite size of the tip. In this work, geometric approaches for the determination of critical sizes of TiO2 anatase bipyramids and nanosheets are described. An uncertainty budget is estimated for each nanoparticle size with the aim of assessing the different sources of error to obtain a more reliable and consistent result. The combined standard uncertainties are respectively less than 5% and 10% of the dimensions of bipyramids and nanosheets. Due to the stability and monomodal distribution of their critical sizes, bipyramids and nanosheets are suitable to apply as candidate reference materials at the nanoscale. Moreover, quantitative measurements of shape and texture descriptors are discussed in order to understand the quality of the synthetized batch