Mesoporous materials endowed with photoluminescence property upon functionalization have potential in many fields such as non-toxic, stable sustained drug storage/release [1,2]. Especially red emitting phosphors prepared with Eu3+ ions have attracted much attentrion in the technological applications. In this study, we aimed at obtaining luminescent CaMO4:Eu@MCM-41 composites via solgel process. The composites thus prepared were characterized via XRD, FT-IR, SEM-EDX, N2 adsorption/desorption analysis, PL and TL spectra. In order to determine the optimum synthesis conditions thermal analysis studies of the initial reactants was made via TG/DTA combined system. A three step decomposition is observed in the DTG curve presented in Figure 1. The first decomposition occurs in the temperature range 450-544 oC, while the second step is observed in the range 544-722 oC and the third step occurs in the range 722-1002 oC. In the temperature range 251002 oC a total weight loss of 18.58 % was observed. Above 1050 oC no weight loss was observed. The mentioned temperatures are the temperatures when phase transitions start and the synthesis were carried out at these temperatures. Figure 1. TG/DTA curves of the initial mixtures of CaMO4