Methodology to evaluate the uncertainty associated with nanoparticle dimensional measurements by SEM

Abstract

The scanning electron microscopy (SEM) technique is widely used for the characterizing of nanoparticle (NP) size, but very few papers deal with NP dimensional metrology. This article reports on a methodology with which to evaluate the uncertainty budget associated with the measurement of the mean diameter of a standard silica NP population by SEM. In this context, the effects of potential error sources have been evaluated though a metrological qualification of the instrument. The measuring method, consisting of determining the area equivalent diameter taken at middle height (Deq-FWHM), has been tested on a reference silica NP with an indicative certification value given by SEM/TEM (number-based modal diameter). Because agglomeration phenomena can cause measurements errors, semi-automatic homemade software has been employed to build the diameter distribution histogram, selecting only isolated particles. Finally, an uncertainty budget, including the main experimental components, has been established for the mean diameter measurement of this silica NP population. The main contributors to this uncertainty budget are the resolution linked to the dimension of the electron beam diameter at the focal plane, the calibration uncertainty on reference NPs, and the measurement repeatability.