A method is described for the preparation of hybrid organic/inorganic structures where the inorganic component comprises semiconductor nanoparticles aligned in periodic layers within three-dimensional (3-D) crystalline powders and Langmuir−Blodgett (LB) films. The preparation process comprises the organization of metal ions in the form of periodic arrays within 3-D crystals or the LB films, followed by a topotactic gas/solid reaction. The method is illustrated for the organization of CdS nanoparticles within alkanoic acids. The order of the nanoparticles is achieved by introducing site directing nucleation centers of Cd thioalkanoates within Cd alkanoates, in the form of solid solutions. The formed particles are attached to the organic matrix via −C(O)S−Cd−S− bonds. The structure of those supramolecular architectures has been characterized by a variety of complementary methods, including transmission electron microscopy (TEM) and electron diffraction (ED), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and other spectroscopic measurements.

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Identification of the phase transition (see Figure) that occurs at the early stages of the topotactic transformation of Langmuir–Blodgett films of Cd or Pb behenate and arachidate with H2S has led to clarification of the structures of the hybrid films, previously in question. The ordered phase is stabilized by the addition of thio‐carboxylic acids to the system.