Within the European iMERA-Plus project 'Traceable Characterisation of Nanoparticles' various particle measurement procedures were developed and finally a measurement comparison for particle size was carried out among seven laboratories across six national metrology institutes. Seven high quality particle samples made from three different materials and having nominal sizes in the range from 10 to 200 nm were used. The participants applied five fundamentally different measurement methods, atomic force microscopy, dynamic light scattering (DLS), small-angle x-ray scattering, scanning electron microscopy and scanning electron microscopy in transmission mode, and provided a total of 48 independent, traceable results. The comparison reference values were determined as weighted means based on the estimated measurement uncertainties of the participants. The comparison reference values have combined standard uncertainties smaller than 1.4 nm for particles with sizes up to 100 nm. All methods, except DLS, provided consistent results.
Six European National Measurement Institutes (NMIs) have joined forces within the European Metrology Research Programme funded project NANOTRACE to develop the next generation of optical interferometers having a target uncertainty of 10 pm. These are needed for NMIs to provide improved traceable dimensional metrology that can be disseminated to the wider nanotechnology community, thereby supporting the growth in nanotechnology. Several approaches were followed in order to develop the interferometers. This paper briefly describes the different interferometers developed by the various partners and presents the results of a comparison of performance of the optical interferometers using an x-ray interferometer to generate traceable reference displacements.
The ability to measure step height and to calibrate step height artefacts is of vital interest in nanometrology. On that score the WGDM7 decided in 1998 to include measurements of step heights in a series of comparisons on the field of nanometrology.The comparison about step height (NANO2) started in September 2000 with the Physikalisch-Technische Bundesanstalt (PTB) as pilot laboratory. Fourteen national metrology institutes worldwide participated in this comparison. A set of five step height standards in the range from 7 nm to 800 nm was used for the comparison. The lateral size of the structures of the step height standards was chosen so that the height could be measured by different types of instruments, for example, interference microscopes, stylus instruments and scanning probe microscopes (SPM). The reference values were calculated as the weighted mean of all measurements that fulfilled the En < 1 criteria.Most of the results were in good agreement with the reference values. It is noticeable that the results obtained by different types of instruments are quite compatible. Also this comparison is the first comprehensive test of the reliability of SPM and their suitability for traceable measurements of step heights. Further it was shown that today step heights on samples can be measured with uncertainties in the sub-nanometre range. Differences in the calculation of the uncertainty depend on the types of instruments and on the users. For each class of instrument, e.g. SPM, it would be meaningful to homogenise these models. Hence the results of this comparison are of great importance in many respects.Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by the CCL, according to the provisions of the Mutual Recognition Arrangement (MRA).
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.
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