Abstract The development of methods for characterising nanoparticles (NPs) at the nanometric scale is a major challenge facing metrology researchers today. The characterisation of the crystal structure of NPs for regulatory purposes is urgent as mixtures of NPs are frequently found in consumer products and this physicochemical parameter contributes to the understanding of potential health and environmental risks. Using the methods currently available, NPs cannot be individually identified and their size distribution cannot be correlated to crystallographic phases. Instead, a general identification of crystallographic phases is possible. New methods must be developed that identify individual particles on the nanoscale. This paper introduces transmission Kikuchi diffraction, an electron backscattered diffraction (EBSD) technique as a method for comprehensively characterizing a mixture of iron oxide NPs by crystal structure. After identifying the crystal structure of three different iron oxide powders using x-ray Diffraction, the samples were characterised by TKD. The results underline the relevance of TKD, which has sufficient spatial resolution to determine the crystal structure of individual NPs. This study also demonstrates the possibility of electron backscattered diffraction analysis on unpolished samples, something atypical for EBSD and TKD. The powders were then mixed and the individual NPs were correctly identified in a scanning electron microscope (SEM) using TKD. The results show that TKD can be used to correctly identify and classify NPs within a mixture and can be combined with SEM imaging to build size distribution histograms according to the NP crystal structure.
Read full abstract