Two nanostructured Al–Cu–Fe alloys, Al64Cu24Fe12 and Al62.5Cu25.2Fe12.3, have been studied. Icosahedral quasicrystalline(w) Al64Cu24Fe12 and crystalline cubic(b) Al62.5Cu25.2Fe12.3cylindrical ingots were first produced using normal casting techniques. High-energy mechanical milling was then conducted to obtain w icosahedral and b intermetallic nanostructured powders. Electrochemical impedance spectroscopy, linear polarization resistance, and potentiodynamic polarization were used to investigate the electrochemical corrosion characteristics of the powders in solutions with different p H values. Current density(icorr), polarization resistance(Rp), and impedance modulus(|Z|) were determined. The results showed that regardless of p H value, increasing the solution temperature enhanced the corrosion resistance of the both phases. However, the electrochemical behavior of the w phase indicated that its stability depends on the submerged exposure time in neutral and alkaline environments. This behavior was related to the type of corrosion products present on the surfaces of the particles along with the diffusion and charge-transfer mechanisms of the corrosion process. Two nanostructured Al-Cu-Fe alloys, Al64Cu24Fe12 and Al62.5Cu25.2Fe12.3, have been studied. Icosahedral quasicrystalline (w) Al64Cu24Fe12 and crystalline cubic (b) Al62.5Cu25.2Fe12.3cylindrical ingots were first produced using normal casting techniques . High-energy mechanical milling was then conducted to obtain w icosahedral and b intermetallic nanostructured powders. Electrochemical impedance spectroscopy, linear polarization resistance, and and potentialodynamic polarization were used to investigate the electrochemical corrosion characteristics of the powders in solutions with different p H values. Current density (icorr), polarization resistance (Rp), and impedance modulus (| Z |) were determined. The results showed that regardless of p H value, increasing the solution temperature enhanced the corrosion resistance of the both phases. However, the electrochemical behavior of the w phase indicated that its stability depends on the submerged exposure time in neutral and alkaline environments. This behavior was related to the type of corrosion products present on the surfaces of the particles along with the diffusion and charge-transfer mechanisms of the corrosion process.