We report here the preparation of luminescent organosilica microcrystals with rectangular-plate morphology by a facile method of reacting silylated β-diketone with lanthanide ions under reflux without any structure-directing agent. Factors affecting the formation of the morphology including reaction temperature and the molar ratio of lanthanide/β-diketone are discussed. FTIR, SEM, XRD, 29Si solid-state NMR spectroscopy and photoluminescence spectroscopy were employed to characterize the obtained microcrystals. Photoluminescence studies show the luminescence of the material is of high monochromatic purity. The 5D0 quantum efficiency of Eu3+ ions was estimated based on the decay time Eu3 + 5D0 excited level and the emission spectrum of the organosilica microcrystals.
