The most widely used hydrogen evolution electrocatalyst for alkaline electrolyzer applications is Ni. However, in order to achieve desired rates of hydrogen generation, large amounts of Ni are required. High surface area Ni electrocatalysts are typically obtained via the caustic leaching of Ni-Al mixtures to obtain Raney Ni. While this process is relatively inexpensive, thick electrodes are needed to ensure enough active surface areas. In this work, an alternative approach for the synthesis of unsupported high-surface-area Ni-based electrocatalysts via spray pyrolysis will be presented. This versatile technique allows the fine-tuning of particle morphology for controlled synthesis of materials with high purity and uniform composition. Furthermore, the promotion effect of rare-earth metal oxides (REO) on the electrochemical activity of Ni electrocatalysts will be studied for rare-earth atomic compositions of 0-10%. Increased surface area of Ni-REO electrocatalysts will be obtained by producing a solute concentration gradient using low melting point precursors, resulting in hollow catalyst particles during the evaporation process. Synthesized catalyst materials will be characterized using XRD for crystallography and phase composition, XPS for elemental catalyst surface composition, electron microscopy (SEM, TEM) for micro and nano-sized morphology, and pore size analysis (BET and PSD). Physical/chemical characterization will be correlated to the observed electrocatalytic activity for the hydrogen evolution reaction (HER) in alkaline electrolytes to better understand the co-catalyst effect of REO on the Ni HER activity.