Impact of thermal treatment on halloysite nanotubes: A combined experimental-computational approach

: Halloysite nanotubes (HNTs) are naturally occurring aluminosilicate minerals, known for their unique tubular structure, which have garnered significant interest for a wide range of applications. This study explores the morphological changes of HNTs when subjected to thermal treatment ranging from 25 °C to 1100 °C using a combination of experimental characterization techniques and molecular dynamics simulations. Techniques such as solid-state NMR (SSNMR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET) surface area measurements, and Fourier Transform Infrared Spectroscopy (FT-IR) were employed to analyse the structural evolution. The results reveal two major transitions: the first occurring between 400 and 500 °C, corresponding to the release of intercalated water and partial distortion of the HNT structure, and the second occurring between 900 and 1000 °C, marked by the collapse of the tubular structure and the exposure of alumina on the surface. These findings provide significant insights into the thermal stability of HNTs, informing future applications, especially in high-temperature environments.