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This invention prepares photoreactive TiO2 nanoparticle coatings through layer-by-layer (LBL) assembly with polyhedral oligomeric silsesquioxane (POSS) molecules on polymer electrospun fibers. In order to increase the efficiency of the TiO2 photocatalysis, fibers with a high surface to volume ratio are electrospun from various polymer solutions and subsequently coated with TiO2 nanoparticles using LBL assembly. Using the electrospinning technique, many different polymers can be formed to create the high specific area substrate, and the flexibility of the polymer fiber is retained after TiO2 LBL nanoparticle coating. Assembly of the TiO2 nanoparticle coating with cationic POSS molecules is used to protect substrates under UV photocatalysis condition , and thus, mitigate concerns about the degradation of the substrate under severe photocatalysis conditions by increasing the number of inert coating layers using the  TiO2 / POSS NH3+ electrolyte nanoparticle pair.