Recently, using eco-friendly controlling methods against pests has been getting great attention. Therefore, this study aimed to assess synthesis of two different phases of nano aluminum oxide, alpha and Gamma, (α- and γ-Al₂O₃ NPs) from wastes. Additionally, evaluate them to control stored product mites, Mycetoglyphus fungivorus, and Caloglyphus mycophagus, and the fungi Aspergillus flavus, Alternaria sp., and Fusarium oxysporum. Two phases of Al₂O₃ NPs were synthesized in acidic and basic media and characterized using the field emission scanning electron microscope (FESEM), energy dispersive X-ray spectroscopy (EDX), ultraviolet-visible (UV-Vis) and thermo gravimetric analysis (TGA). Mortality percentages of mites were evaluated at concentrations of 10, 30 and 60 ppm after 1, 2, 3 and 4 days. The growth of fungi was assessed to determine the fungicidal concentrations in PDB cultures by Mycelium Dry Weights Method. The study confirmed the formation and thermal stability of α- and γ-Al₂O₃ NPs using FESEM, UV-Vis and TGA. The average particle size of α-Al₂O₃ is 4–10 nm and for γ- Al₂O₃ is 14–30 nm. Both phases were toxic to tested stages of mites. Increasing concentration and exposure time, results in increased mite mortality rates. γ-Al₂O₃ NPs were more efficient than α-NPs post initial exposure, then all through time both have the same effect. The female's fecundity was significantly influenced. Tested eggs did not hatch at all. The toxic activity remained strong after 1, 2, and 3 months of exposure. The SEM images revealed a strong adhesive of α- and γ-NPs which were visibly bonded to various areas of dead mite females. γ-Al₂O₃ showed antifungal activity more than the α-NPs. Concentrations of fungicides depended on the fungal strain sensitivity. It has been concluded that α- and γ-Al₂O₃ NPs are efficient environmentally friendly agents against the proliferation of storage mites and mycotoxin producing fungi.