Abstract Superhard materials AlMgB 14 – x TiB 2 disks were synthesized by a two-step heat-treatment method. In the first step, AlMg 6 B 14 – x TiB 2 disks were fabricated by uniformly mixed Mg, B, Al powders and different contents Ti powder, and then AlMg 6 B 14 – x TiB 2 disks were heated at 850 °C for 2 h in closed argon atmosphere. In the second step, AlMg 6 B 14 – x TiB 2 disks were sintered at 1050 °C for half an hour in vacuum, then target AlMgB 14 – x TiB 2 disks were obtained. The phase, microstructure and superconductivity were characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM) and superconducting quantum interference device (SQUID). The nano-scale TiB 2 particles as the second phase induced by Ti doping are uniformly distributed in the sample matrix. The results reveal that the stepwise synthesis method can produce practical AlMgB 14 –TiB 2 materials.