oxidation methods. In particular, a zinc nanobranched structure is deposited by radio-frequency magnetron sputtering on conductive substrates. Then impregnation of the samples in an antimony acetate solution is performed at different times (2 and 4 h) at room temperature. It has to be noted that longer times produce however an appreciable and even complete dissolution of the zinc material in the Sb acetate solution (at 8 and 16 h, respectively), whereas very short impregnation times (30 min) did not result in a signifi cant doping. Therefore, it resulted that a reasonable impregnation time for inducing a satisfying doping level, without altering the morphological properties of the investigated materials, lies in the range of 2-4 h. The impregnation is then followed by a thermal oxidation at 380 °C, having the dual function to oxidize Zn to ZnO and successfully promote the insertion of Sb in the wurtzite structure, leading to doped ZnO at different ratios depending on the impregnation time. This doping results in a p-type conductive structure and we show that ZnO:Sb nanobranched fi lms can be successfully used as piezoelectric nanogenerators, while the presence of ferro electricity, together with a nonzero spontaneous polarization, is found to give rise to the ferroelectric-photovoltaic effect, [ 11 ] which is here reported for the fi rst time for a ZnObased nanomaterial.The highly nanoporous morphology of the starting Zn layer is shown in Figure S1 (Supporting Information). We take advantage of such a high porous volume and exposed surface area to succeed in the optimal impregnation of the Zn materials with the Sb-precursor solution. Figure 1 a shows the surface morphology of pristine ZnO sample, after calcination of Zn grown on a fl uorine-doped tin oxide (FTO)/glass substrate, and considered the reference sample of this work. The surface is mainly formed by elongated and branched nanostructures, giving rise to a nanoporous network (surface area 14 m 2 g â1 , pore volume 0.095 cm 3 g â1 ). [ 7b ] The presence of a similar highly porous and nanobranched morphology (with a pore volume variation of about ±5% with respect to pristine ZnO fi lm) is also visible in the ZnO:Sb fi lms (Figure 1 b,c) and it is found to be independent from the impregnation time and not signifi cantly altered by doping and thermal processes. Further insight into the morphology of the nanoporous fi lms is given by high-resolution transmission electron microscopy (HRTEM) images (from Figure 1 d-f), showing that the nanobranches are actually constituted by grains smaller than 50 nm for both the pristine and the impregnated samples. Moreover, it can be inferred from HRTEM and fast Fourier transform (FFT) image processing that the grains are single crystals with hexagonal Wurtzite ZnO nanomaterials are widely investigated thanks to the copresence of several unique physical properties like their semiconducting and piezoelectric behaviors. Among all the different morphologies, high-surface area nanostructures are of great interest, such as ZnO n...