Energy-dispersive X-ray (EDX) analysis is an elemental analysis technique associated with Field Scanning Electron Microscopy (FESEM); it is frequently used in material science and engineering. EDX analysis enables both qualitative and quantitative studies to be carried out for a variety of applications. In this study, aluminum and fluorine (Al, F) co-doped zinc oxide nanoparticles were grown using the sol–gel route via the spin-coating method with various (Al, F) contents (1 at.%, 1 at.%), (3 at.%, 3 at.%), (5 at.%, 5 at.%), and (7 at.%, 7 at.%). The as-grown samples were characterized by energy-dispersive X-ray (EDX) and Scanning Electron Microscopy (FESEM) techniques. The results revealed that the nanoparticles have uniform morphology and hexagonal structure with a homogenous distribution. We can observe the incorporation of Al and F into the zinc oxide lattice when (Al, F) content is (1 at.%, 1 at.%) and (3at.%, 3 at.%) while the presence of Al and F peaks in the spectrum of EDX results was demonstrated in the two dopants with (Al, F) content (5 at.%, 5 at.%) and (7 at.%, 7 at.%), indicating the film's microstructure quality degradation. Grain sizes ranged from 10 to 13 nm. In conclusion, simultaneous co-doping improved the microstructure of FAZO nanoparticles when the (Al, F) content was (1 at.%, 1 at.%) and (3 at.%, 3 at.%); thus, EDX can be considered as a useful technique in all research works that require element determination.