The development of alternative processes for fabricating functional semiconductor nanomaterials and precisely controlling their properties is of significant scientific interest across various domains. A key driver is the energy transition, where the growing demand for semiconductors is challenged by the limited availability of rare-earth-based materials, which are essential for high-efficiency solar cells and sustainable electronics. Zinc oxide (ZnO), a well-established wide-bandgap semiconductor, can be transformed into a transparent conductive oxide (TCO) through aluminum doping. As a result, aluminum-doped ZnO (AZO) presents a cost-effective alternative to indium tin oxide (ITO) for transparent electrode applications. To investigate the properties of AZO nanoparticles during sol-gel synthesis, a multiscale characterization approach was developed. A combination of small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), energy-dispersive X-ray spectroscopy (EDX), and image analysis, facilitated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and high-angle annular dark-field imaging (HAADF-STEM), along with gravimetric analysis and UV-Vis spectroscopy, provided comprehensive insights into AZO morphology and material properties. This included the hierarchical evolution of particle size, number and mass concentration, AZO composition, morphology, and bandgap. The complete experimental dataset is openly published to support further research and development in the field.

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