Duplex stainless steel is a structural material that is highly used in nuclear power plants, especially in the reactor core components and pipelines. Long-term exposure of duplex stainless steel in a high-temperature working environment will cause thermal aging embrittlement. Material deterioration will affect the long-term reliability of nuclear power plants. In this work, we used two different ultrasonic techniques, namely Laser Ultrasound Technique (LUT) and Non-linear Ultrasonic Technique (NUT) for measuring the material properties. The LUT has unique advantages such of being non-contact, non-destructive, and remotely operable, while NUT has considerable measurement sensitivity to the microstructure changes of materials. Therefore, this research mainly focused on duplex stainless steel after the heat aging treatment. The changes in the material properties of the duplex stainless steel after the heat aging treatment were investigated by ultrasonic testing and traditional material testing methods. The results of this study show that the thermal aging with higher duration, the ferrite phase decomposes into Cr-rich αˊ-phase and Fe-rich α-phase. The hardness of both the austenite iron phase and the ferrite iron phase increase with the increase in heat aging time. The phase velocity of duplex stainless steel increases significantly up to a heat aging of 2400 h, and then the phase velocity decreases significantly. After thermal aging treatment at different times, the non-linear factor did not change significantly due to the hardness changes. The non-linear response caused by the heat aging treatment of duplex stainless steel is minimum.