Spray pyrolysis typically produces hollow particles when the particles are larger than about 2 microns. In this work, a scalable spray pyrolysis process was developed for the production of electrochemically active materials in a way that overcomes hollow sphere formation. With this new slurry spray pyrolysis process particles greater than 6 μm have been successfully produced with a solid, yet porous interior morphology. Results indicate that the process shows great potential for the production of high quality, electrochemically active materials, as demonstrated by the electrochemical performance of layered Li1.2Mn0.54Ni0.13Co0.13O2 materials. The materials are phase pure, as observed by powder X-ray diffraction (XRD), and discharge capacities greater than 200 mAh g−1 after 100 cycles at C/3 rate (where 1 C = 200 mAh g−1) are consistently obtained. The standard deviation in discharge capacity for 5 batches of material produced under identical conditions was 11 mAh g−1. These promising electrochemical results were obtained at a scale of 50 g h−1 and with minimal process optimization, indicating the potential for commercial scale production.