Abstract <p>This paper presents the synthesis of layered complex carbide of the composition (Cr,V)C using reactive spark plasma sintering (SPS-RS) and hydrothermal acid etching. Using SEM and TEM, the macrostructure and nanostructure at each stage of MAXene synthesis was studied in detail. The presence of characteristic features of the formation of two-dimensional carbide in the form of particles and fragments of a multilayer structure at the macro- and nanolevel was confirmed. Using EDS and powder X-ray diffraction, the elemental and phase composition of the samples was studied. As a result, it was found that the expected MAX-phase Cr₂VAlC₂ in the composition of the sample obtained by SPS is absent. At the same time, a phase of mixed bimetallic carbide (Cr,V)C was detected at all stages of synthesis, for which the crystal lattice parameters, including the unit cell volume, change significantly after acid etching. Obvious changes in the bulk and crystalline structure of (Cr,V)C correspond to the formation of two-dimensional nanoparticles in the synthesized material. The magnetic characteristics study showed that all samples have magnetic hysteresis with relatively low values of coercivity and remanence to saturation magnetization ratio. Low-temperature measurements showed a slight increase in magnetic moment with decreasing temperature for the sample obtained under reaction SPS conditions before acid etching in HF, without significant changes in magnetic behavior of the samples.</p>