Metal–organic framework (MOF) derived materials have shown great potential for energy storage applications, due to their high porosity and large surface area. However, synthesizing these materials is challenging due to the effect of heat treatment factors on the resulting compound. This study reports the synthesis of a trimetal-organic framework, MgNi-ZIF-67, by incorporating Ni and Mg ions into the ZIF-67 structure. Subsequent carbonization of this compound resulted in a novel trimetallic oxide–carbon nanocomposite, (Mg, Ni, Co)3O 4 @C. We explored the effects of three distinct heat treatment protocols on the microstructural and electrochemical properties of the resulting nanocomposite as lithium-ion battery anode. The sample obtained through carbonization at a low heating rate (Z2) exhibited superior electrochemical performance, delivering an initial capacity of 580.2 mAh g –1 and retaining 480.1 mAh g –1 after 100 cycles at 500 mA g –1 . Notably, Z2 showed a capacity of 204.4 mAh g –1 even at a high current density of 2000 mA g –1 . The superior electrochemical stability of Z2 is ascribed to the preservation of the MOF’s carbon structure during carbonization under optimal atmospheric conditions and heating rate. This facilitated the formation of trimetallic oxide nanoparticles (15 nm) were evenly distributed within the carbon matrix. This led to a porous structure with a high specific surface area of 198.62 m 2 g−1 , making it suitable for lithium-ion battery anodes. This study highlights the importance of heat treatment parameters in enhancing the performance of MOF-derived nanocomposites for use in the area of energy storage.

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