Zinc oxide nanostructures such as nanosheets (NS) and nanoflowers (NF) were obtained by a facile hydrothermal synthesis using zinc chloride (ZnCl ₂ ) as precursor with low molar concentrations and a short synthesis time (2 h) at 200 °C. By means of X-ray diffraction and Raman spectroscopy measurements, the wurtzite-type ZnO structure was confirmed with high crystalline quality. SEM micrographs showed the influence of ZnCl ₂ concentration on ZnO morphology; ZnO NF were obtained at low concentrations (0.02 and 0.05 M), while ZnO NS were seen for higher concentrations (0.2–0.6 M) and their thicknesses can be estimated from 15 to 60 nm. In addition, TEM images showed a large number of pores with sizes below 15 nm in both ZnO nanostructures. Raman and photoluminescence displayed the surface defects density for ZnO nanostructures. Raman spectra showed the E ₁ (LO) mode localized at ∼581 cm ⁻¹ , associated with oxygen vacancies and zinc interstitials, being more intense for ZnO NF, while photoluminescence results showed a strong yellow-orange emission (centered from 587 to 618 nm) relative to UV emission, being more intense for ZnO NF. These properties reveal further potential for high performance luminescent devices based on ZnO NF and NS.

Surface enhanced Raman spectroscopy (SERS) is considered a versatile and multifunctional technique with the ability to detect molecules of different species at very low molar concentration. In this work, hierarchical ZnO microspheres (ZnO MSs) and Ag/ZnO MSs were fabricated and decorated by hydrothermal and photodeposition methods, respectively. For Ag deposition, precursor molar concentration (1.9 and 9.8 mM) and UV irradiation time (5, 15, and 30 min) were evaluated by SEM, TEM, X-ray diffraction and Raman spectroscopy. X-ray diffraction showed a peak at 37.9° corresponding to the (111) plane of Ag, whose intensity increases as precursor concentration and UV irradiation time increases. SEM images confirmed the formation of ZnO MSs (from 2.5 to 4.5 µm) building by radially aligned two-dimensional ZnO nanosheets with thicknesses below 30 nm. The Raman spectra of Ag/ZnO MSs exhibited a vibration mode at 486 cm⁻¹ which can be directly associated to Ag deposition on ZnO MSs surface. The performance of SERS substrate was evaluated using rhodamine 6G. The SERS substrate grown at 9.8 mM during 30 min showed the best SERS activity and the ability to detect methylene blue at 10⁻⁹ M.