a series of M 2 (dobdc) materials (MOF-74 or CPO-27; M = Mn, Co, Ni, Cu, Zn, etc, dobdc 4-= 2,5-dioxide-1,4-benzenedicarboxylate), which are stable in various solvents, have been extensively studied. [10,11] MOF-74 materials consist of 11 Å-wide 1D hexagonal channels, which is beneficial to improve electrolyte permeability and reduce steric hindrance for fast electron transfer. [12,13] Furthermore, MOF-74 materials have a high density of potential open metal sites in the framework, and the unique advantage can replace metal nodes without destroying the basic framework structure of MOF crystals, which makes it promising to design stable bi/ multimetallic MOF topologies. [14] However, obtaining MOF-74 materials with high capacity and high energy density remains a challenge due to the limitation of the single metal active site.It has been reported that metal-ion doping can adjust the electronic structure and enhance the synergy, thereby enhancing the electrochemical performance. [15,16] The representative synthesis strategies of multimetallic MOFs include one-pot synthesis and post-synthetic strategy. [17][18][19][20] Li et al. [21] reported the direct synthesis strategy of multimetallic MnM-MIL-100 nano-octahedra with an excellent electrochemical performance in Li-S batteries. Choi et al. [22] summarized a series of multimetal mixed MOF composites based on MOF-74, which showed more satisfactory performance than unmixed ones in supercapacitors. The bi/multimetallic MOF-74 materials possess abundant potential Lewis acidic active sites, [21,23] providing the possibility to improve electrochemical performance, especially when used as cathode materials for aqueous nickel-zinc batteries (NZBs).Among various aqueous zinc-based batteries (such as Zn-Mn, Zn-Co, Zn-Ni batteries, etc.), NZBs exhibit high specific capacity, high safety, and high operating voltage of ≈1.75 V, based on the high redox potential of Ni 2+ /Ni 3+ (0.49 V versus (vs) standard hydrogen electrode (SHE)) and the low redox potential of Zn(OH) /Zn 4 2− (−1.26 V vs SHE) in alkaline electrolyte, which makes it competitive and attractive for nextgeneration high-energy-density energy-storage devices. [24][25][26] In addition, designing electrodes with high mass loading of active materials can increase the areal energy density of the NZBs. [27][28][29] Currently, the practical application of aqueous Limited by single metal active sites and low electrical conductivity, designing nickel-based metal-organic framework (MOF) materials with high capacity and high energy density remains a challenge. Herein, a series of bi/multimetallic MOF-74 family materials in situ grown on carbon cloth (CC) by doping M x+ ions in Ni-MOF-74 is fabricated: NiM-MOF@CC (