An electron microscopy three-dimensional characterization of titania nanotubes

Microsc Res Tech. 2019 Mar;82(3):173-177. doi: 10.1002/jemt.23093. Epub 2018 Oct 8.

Abstract

To characterize complex, three-dimensional nanostructures, modern microscopy techniques are needed, such as electron tomography and focused ion beam (FIB) sectioning. The aim of this study was to apply these two techniques to characterize TiO2 nanotubes in terms of their size, shape, volume, porosity, geometric surface area, and specific surface area (SSA). For these experiments, titania nanotubes were fabricated by means of the electrochemical oxidation of titanium at a voltage of 20 V for 2 hr followed by heat treatment at 450°C for 3 hr to change the amorphous structure into a crystalline anatase structure. The quantitative data obtained from the FIB and electron tomography reconstructions show a high similarity in porosity and some differences in SSA. These might be the result of differences in resolution between the two reconstruction techniques.

Keywords: 3D structure; FIB sectioning; electron tomography; titania nanotubes.