Transformation of Amorphous Terbium Metal-Organic Framework on Terbium Oxide TbO x (111) Thin Film on Pt(111) Substrate: Structure of Tb x O y Film.

The present study is focused on the synthesis and structural properties of amorphous terbium metal-organic framework thin film (TbMOF-TF) and its transformation to terbium oxide by pyrolysis at 450 °C in the air. The crystalline (cTbMOF) and amorphous (aTbMOF) films were prepared by solvothermal synthesis using different amounts (0.4 and 0.7 mmol) of the modulator (sodium acetate), respectively. The powders were characterized by differential scanning calorimetry (DSC), thermogravimetry (TG), Fourier transform infrared (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM). The varied chemical composition of the surface of TbMOFs and Tb x O y was investigated by X-ray photoelectron spectroscopy (XPS). X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed that aTbMOF had been fully transformed to a Tb 4 O 7 phase with a cubic crystal structure at 450 °C. The amorphous aTbMOF-TF film was prepared by dropping a colloidal solution of amorphous precursor nanocrystals on the SiO 2 /Si substrates covered with Pt as an interlayer. XPS confirmed the presence of Tb in two states, Tb 3+ and Tb 4+ . The amorphous film has a rough, porous microstructure and is composed of large clusters of worm-like particles, while terbium oxide film consists of fine crystallites of cubic fluorite cF-TbO x , c-Tb 4 O 7, and c-Tb 2 O 3 phases. The surface topography was investigated by a combination of confocal (CM) and atomic force microscopy (AFM). The amorphous film is porous and rough, which is contrast to the crystalline terbium oxide film.