Crystalline Ni2B, Ni3B, and Ni4B3 are synthesized by a single-step method using autogenous pressure from the reaction of NaBH4 and Ni precursors. The effect of reaction temperature, pressure, time, and starting materials on the composition of synthesized products, particle morphologies, and magnetic properties is demonstrated. High yields of Ni2B (>98%) are achieved at 2.3–3.4 MPa and ~670 °C over five hours. Crystalline Ni3B or Ni4B3 form in conjunction with Ni2B at higher temperature or higher autogenous pressure in proportions influenced by the ratios of initial reactants. For the same starting ratios of reactants, a longer reaction time or higher pressure shifts equilibria to lower yields of Ni2B. Using this approach, yields of ~88% Ni4B3 (single phase orthorhombic) and ~72% Ni3B are obtained for conditions 1.9 MPa < Pmax < 4.9 MPa and 670 °C < Tmax < 725 °C. Gas-solid reaction is the dominant transformation mechanism that results in formation of Ni2B at lower temperatures than conventional solid-state methods.
Single Step Process for Crystalline Ni-B Compounds