A206–Al2O3 metal matrix nanocomposite (MMNC) is a promising high performance material with potential applications in various industries, such as automotive, aerospace, and defense. Al2O3 nanoparticles dispersed into molten Al using ultrasonic cavitation technique can enhance the nucleation of primary Al phase to reduce its grain size and modify the secondary intermetallic phases. To enable a scale-up production, an effective yet easy-to-implement quality inspection technique is needed to effectively evaluate the resultant microstructure of the MMNCs. At present the standard inspection technique is based on the microscopic images, which are costly and time-consuming to obtain. This paper investigates the relationship between the ultrasonic attenuation and the microstructures of pure A206 and Al2O3 reinforced MMNCs with/without ultrasonic dispersion. A hypothesis test based on an estimated attenuation variance was developed and it could accurately differentiate poor samples from good ones. This study provides useful guidelines to establish a new quality inspection technique for A206–Al2O3 nanocomposites using ultrasonic nondestructive testing method.