A promising Li-ion battery anode material, nanostructured ZnCo2O4 spinel, is tailored by solution combustion synthesis to explore how reaction conditions can be tuned to enhance electrochemical performance. A strategy of using glycine and citric acid as fuels, ammonium nitrate as gas generating agent, and optimized fuel to oxidizer ratio results in a mild volume combustion mode with significant weight loss by gas evolution occurring during calcination to mitigate particle sintering. This yields a mesoporous product structure with a tap density of 1.48 g cm–3, which accommodates volumetric changes during lithiation, resulting in a high stable capacity of 1000 mAh g–1 (C/2 rate) and 950 mAh g–1 (1 C rate) at 22 °C after initial formation cycles. This study demonstrates that with the use of mixed fuels, gas generating additives, and appropriate fuel to oxidizer ratio, ZnCo2O4 material synthesized by the efficient, one-step solution combustion synthesis method can be tuned to provide excellent electrochemical...