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The effect of hydration procedure of fumed silica precursor on photoluminescent properties of carbonized silica (SiO2:C) nanocomposite after chemo/thermal treatments is studied. Main structural effect is the formation of chemical bonding of phenyl groups to silica surface via multiple CSiO bonding bridges. Synthesized samples demonstrate very broad photoluminescence (PL) bands in near ultraviolet and visible ranges with maximum intensity dependent on temperature of thermal annealing. Two main trends in luminescence properties are: 1) hydration-induced blue shift of PL in comparison with PL of unhydrated series; 2) red shift of PL bands with increasing synthesis temperature regardless hydration procedure. Temperature dependent evolution of light emission bands is discussed in terms of surface carbon nanoclusters formation and aggregation processes. It is assumed that blue shift of PL bands in the hydrated series is associated with the decreased surface mobility of carbon atoms and clusters as a result of increased chemical bonding with silica surface that slows down carbon thermally stimulated clusterization/aggregation processes.