The M-doped (M=Y and Eu) microporous zirconosilicate AV-3 materials, possessing the structure of mineral petarasite and with Zr/M ratio of 4, have been prepared via hydrothermal synthesis. The structure of these materials contains elliptical channels, running down the b- and c-axes, defined by mixed six-membered rings, consisting of pairs of SiO4 tetrahedra linked by ZrO6 octahedra. There are also six-membered silicate ring channels running parallel to the c-axis. M ions predominantly occupy Zr positions, sitting on the channel surface and making AV-3 a proper system to create new multifunctional photoluminescent material. The solids have been characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), solid-state magic-angle spinning nuclear magnetic resonance (MAS NMR) and photoluminescence spectroscopy.