In Situ High-Temperature Transmission Electron Microscopy Observations of the Formation of Nanocrystalline TiC from Nanocrystalline Anatase (TiO₂)

Abstract

In this work, the high-temperature behavior of nanocrystalline TiO₂ is studied using in situ transmission electron microscopy (TEM). These nanoparticles are made using wet chemical techniques that generate the anatase phase of TiO₂ with average grain sizes of 6 nm. X-ray diffraction studies of nanophase TiO₂ indicate the material undergoes a solid-solid phase transformation to the stable rutile phase between 600° and 900°C. This phase transition is not observed in the TEM samples, which remain anatase up to temperatures as high as 1000°C. Above 1000°C, nanoparticles become mobile on the amorphous carbon grid and by 1300°C, all anatase diffraction is lost and larger (50 nm) single crystals of a new phase are present. This new phase is identified as TiC both from high-resolution electron microscopy after heat treatment and electron diffraction collected during in situ heating experiments. Video images of the particle motion in situ show the nanoparticles diffusing and interacting with the underlying grid material as the reaction from TiO₂ to TiC proceeds.