ZnO nanowalls (NWLs) represent a non-toxic, Earth abundant, high surface-to-volume ratio, semiconducting nanostructure which has already showed potential applications in biosensing, environmental monitoring and energy. Low-cost synthesis of these nanostructures is extremely appealing for large scale upgrading of laboratory results, and its implementation has to be tested at the nanoscale, at least in terms of chemical purity and crystallographic orientation. Here, we have produced pure and texturized ZnO NWLs by using chemical bath deposition (CBD) synthesis followed by a thermal treatment at 300 C. We examined the NWL formation process and the new obtained structure at the nanoscale, by means of scanning and transmission electron microscopy in combination with x-ray diffraction and Rutherford backscattering spectrometry. We have shown that only after annealing at 300 C in nitrogen does the as …