iThe changes in the electronic structure and nature of the chemical bonds due to the ordering of the intercalated atoms inside the van der Waals gap were observed for the first time.

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Our experimental results indicate the formation of extended ordered S–Ti–Se layers (Janus layers) in the Ti­(Se1–x S x )2 system. The presence of these layers is observed as a folding of the typical Fermi surface of TiS2 and TiSe2. High-resolution transmission electron microscopy (HRTEM) allows us to observe these layers by a typical rotation of the moiré fringe images. Analysis of the dependence of the electromotive force of the electrochemical cell on the S:Se ratio, angle-resolved photoelectron spectroscopy, resonant photoelectron spectroscopy, Fermi surface mapping, and HRTEM data allows us to conclude that the structure of the solid solution consists of S–Ti–Se and TiCh2 (Ch = S or Se) Janus layers.