In this work, Mo, Y, Al, and C were used as raw materials to synthesize a novel (Mo_2/3Y_1/3)₂AlC MAX phase by spark plasma sintering (SPS) at 1550 ℃, and the corresponding accordion-like MXene was successfully obtained with a milder chemical etching method. The chemical composition and microstructure of the materials were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and energy dispersive spectrometer (DES). The final product was Mo_1.33CT₂ MXene with functional groups on the surface. At the same time, the electronic structure and electronic properties of the novel (Mo_2/3Y_1/3)₂AlC MAX phase and the corresponding Mo_1.33CT₂ MXene were studied by the first-principles density functional theory. The calculated results show that all of them exhibit metallic properties, which are expected to be applied for energy storage, biosensors and electrocatalysis.