Combined with ultrasonic pulse-echo technique, reflection spectrum analysis was introduced to evaluate TiAl and 40Cr diffusion bonding quality. Frequency dependence of reflection coefficient was used to distinguish perfect bonding from imperfect bonding. It is found that the reflection coefficient from perfect bonding interface does not vary with frequency. When the size of imperfections is much smaller than the wavelength of ultrasound, the reflection coefficient depends on frequency. When the size of imperfections is the same order of or even larger than the wavelength of ultrasound, the reflection coefficient does not exhibit frequency dependence. However the amplitude of imperfect interface is higher than the amplitude of perfect bonding interface. A combination of reflection spectrum analysis and ultrasonic pulse-echo technique provides more accurate information about the bonding quality of dissimilar materials.