The Big Problem of Small Particles:  A Comparison of Methods for Determination of Particle Size in Nanocrystalline Anatase Powders

We compare different methods for particle size determination in nanocrystalline anatase (TiO2) powders: transmission electron microscopy (TEM), nitrogen adsorption measurements, mercury porosimetry, and X-ray diffraction (XRD). The main source of errors in TEM is the sampling of the powder population, whereas in XRD the deconvolution of peak broadening due to instrument, microstrains, and crystalline domain size is delicate and can lead to unreliable results. Different approaches including Scherrer and Williamson−Hall equations are discussed. The presence of mesopores due to agglomerate formation is clearly revealed in adsorption measurements and porosimetry.