In this paper, a room-temperature NO2 sensor based on a polyaniline (PANI)/black phosphorus (BP) composite material was proposed to solve the power consumption problem of traditional metal-oxide sensors operating at high temperatures. PANI was synthesized by chemical oxidative polymerization, whereas BP was synthesized by low-pressure mineralization. The PANI/BP composite materials were prepared via ultrasonic exfoliation and mixing. Various characterization techniques, including scanning electron microscope (SEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS), confirmed the successful preparation of the PANI/BP composites and their excellent structural properties. The sensor demonstrated outstanding gas sensitivity in the NO2 concentration range of 2–60 ppm. In particular, the sensor showed a response exceeding 2200% at 60 ppm NO2 concentration when using a 1:1 mass ratio of PANI to BP in the composite material.
