In this paper we report the midscale synthesis of the monometallic catalyst gamma-Mo2N and bimetallic catalyst Ni2Mo3N/Al2O3 from their corresponding oxide compounds by temperature-programmed reaction in mixtures of H-2 and N-2. The reaction was carried out in a self-designed midscale fluidized bed synthesis apparatus. The apparatus was specifically designed to control the reaction temperature precisely and to remove the generated water efficiently. The operation conditions for the equipment were first settled by synthesizing bulk gamma-Mo2N from MoO3. The Ni2Mo3N/Al2O3 catalyst for hydrogenation of aromatics in oil was synthesized following the same preparation condition. The product was characterized by XRD, BET, SEM, and TEM to obtain its physical information. The chemical content of the catalyst was settled by ICP to analyze the Ni and Mo contents and by a TC-436 nitrogen and oxygen analyzer to analyze the nitrogen content. The obtained bulk gamma-Mo2N was platelet particles and has a specific surface area of 126.7 m(2)/g. The catalyst Ni2Mo3N supported on Al2O3 was striplike crystals, and the chemical content was 5.24 wt % Ni, 12.0 wt % Mo, and 0.63 wt % N.