This article’s objective is the synthesis of new composites based on thermoplastic polyurethane (TPU) and TiO
2 nanowires (NWs) as free-standing films, highlighting their structural and optical properties. The free-standing TPU–TiO
2 NW films were prepared by a wet chemical method accompanied by a thermal treatment at 100 °C for 1 h, followed by air-drying for 2 h. X-ray diffraction (XRD) studies indicated that the starting commercial TiO
2 NW sample contains TiO
2 tetragonal anatase (A), cubic Ti
0.91O (C), and orthorhombic Ti
2O
3 (OR), as well as monoclinic H
2Ti
3O
7 (M). In the presence of TPU, an increase in the ratio between the intensities of the diffraction peaks at 43.4° and 48° belonging to the C and A phases of titanium dioxide, respectively, is reported. The increase in the intensity of the peak at 43.4° is explained to be a consequence of the interaction of TiO
2 NWs with PTU, which occurs when the formation of suboxides takes place. The variation in the ratio of the absorbance of the IR bands peaked at 765–771 cm
−1 and 3304–3315 cm
−1 from 4.68 to 4.21 and 3.83 for TPU and the TPU–TiO
2 NW composites, respectively, with TiO
2 NW concentration equal to 2 wt.% and 17 wt.%, indicated a decrease in the higher-order aggregates of TPU with a simultaneous increase in the hydrogen bonds established between the amide groups of TPU and the oxygen atoms of TiO
2 NWs. The decrease in the ratio of the intensity of the Raman lines peaked at 658 cm
−1 and 635 cm
−1, which were assigned to the vibrational modes E
g in TiO
2 A and E
g in H
2Ti
3O
7 (I
TiO2-A/I
H2Ti3O7), respectively, from 3.45 in TiO
2 NWs to 0.94–0.96 in the TPU–TiO
2 NW composites, which indicates that the adsorption of TPU onto TiO
2 NWs involves an exchange reaction of TPU in the presence of TiO
2 NWs, followed by the formation of new hydrogen bonds between the -NH- of the amide group and the oxygen atoms of Ti
xO
2x-mn, Ti
2O
3, and Ti
0.91O. Photoluminescence (PL) studies highlighted a gradual decrease in the intensity of the TPU emission band, which is situated in the spectral range 380–650 nm, in the presence of TiO
2 NW. After increasing the TiO
2 NW concentration in the TPU–TiO
2 NW composite mass from 0 wt.% to 2 wt.% and 17 wt.%, respectively, a change in the binding angle of the TPU onto the TiO
2 NW surface from 12.6° to 32° and 45.9°, respectively, took place.
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