The water resources are polluted because of the widespread use of dyes in the industry, resulting in a major ecological threat. Among the various water treatment techniques, adsorption and photocatalytic degradation methods are the most preferred owing to their easy applicability, low cost, and high efficiency. Silicon oxycarbide (SiOC), which is a type of polymer-derived ceramic, has the potential to be used in harsh environmental conditions thanks to its strong chemical stability and oxidation resistance, that being said it can also be used as a photocatalyst substrate. Titanium dioxide (TiO2) photocatalysts are extensively used for purification of contaminated waters. And also, TiO2 particles are synthesized with various material groups to investigate the adsorption and photocatalytic effect. In this thesis, initially, submicron/nano SiOC spheres were produced via an oil in water (o/w) emulsion technique by using parameters such as two types of preceramic polymer precursors (silicon oil and resin), mixing types (magnetically and ultrasonically), and different pyrolysis temperature (600-1200 oC). Upon the formation of submicron/nano SiOC spheres, selected samples were impregnated with a different molar of titanium oxide precursor solution (Titanium(IV) n-butoxide (TBT)) and calcined at 450 °C for 4 h. Various amounts of (0-5-10-20 wt.%) TiO2 containing submicron/nano SiOC spheres were produced and then characterized in depth by various techniques. Finally, the effects of pyrolysis temperatures and the amount of TiO2 were investigated in terms of adsorption and photocatalytic performance against aqueous cationic dye (methylene blue) (MB) solution. In the adsorption experiments, pure SiOC submicron/nanospheres (UM1200), pyrolyzed at 1200 oC, showed the best performance at the end of 24 h in the dark with 64% adsorption. In photocatalytic experiments, samples obtained by coating the SiOC substrate produced by pyrolysis at 600 oC with different amounts of TiO2 (UM600T5, UM600T10 and UM600T20) showed 79%, 80%, and 87% photodegradation efficiency.