Copper oxide (CuO), titanium oxide (TiO 2 ), and Cu-doped TiO 2 nanoparticles have been synthesized by pyrolysis of their corresponding precursors initially prepared by precipitation in aqueous solution using A. carambola fruit juice as a natural source of the precipitating agent (oxalate). The precursors were synthesized and characterized by FTIR, TGA, and PXRD. The results revealed that the precursors obtained were CuC 2 O 4 , TiO 2 (OH − ) 2 C 2 O 4 , copper-doped titanium hydroxyl oxalate, and copper titanium hydroxyl oxalate. Complete decomposition for the as-prepared precursors containing titanium ions occurs at 600 ∘ C while impurity free copper oxalate decomposed at 450 ∘ C. The as-prepared precursors were decomposed and calcined at 600 ∘ C for 4 hours and the calcination products were characterized by XRD, SEM, and EDX. The results revealed the decomposition products to correspond to CuO, TiO 2 , Cu 0.131 Ti 0.869 O 2 , and CuO/TiO 2 .