The pursuit of high mass loading metal–organic framework (MOF) materials via a simple method is crucial to achieve high-performance supercapacitors. Herein, an amorphous NiCo-MOF material with a high mass loading of up to 10.3 mg cm⁻² was successfully prepared using a mixed solvent system of ethanol and water. In addition, by adjusting the volume ratio of ethanol to water, amorphous NiCo-MOFs with three different morphologies including nanospheres, nanopores, and ultra-thick plates were obtained. It was found that the different solvent systems not only affected the growth rate of MOFs, but also controlled their nucleation rate by changing the coordination environment of the metal ions, and thus achieved morphology and mass loading regulation, thereby influencing their energy storage behavior. Notably, the optimum NiCo-MOF exhibited the superior specific capacitance of up to 9.7 F cm⁻² (941.8 F g⁻¹) at a current density of 5 mA cm⁻² and high-rate capability of 71.1% even at 20 mA cm⁻². Moreover, the corresponding assembled solid-state supercapacitor exhibited an excellent energy density of 0.65 mW h cm⁻² at a power density of 2 mW cm⁻² and capacity retention of 84.7% after 8000 cycles at 30 mA cm⁻². Overall, this work proposes a feasible and effective strategy to achieve high mass loading NiCo-MOFs, impacting their ultimate electrochemical performance, which can possibly be further extended to other MOFs with superior capacitance.