To apply electrically nonconductive metal-organic frameworks (MOFs) in an electrocatalytic oxygen reduction reaction (ORR), we have developed an ew method for fabricating various amounts of CuS nanoparticles (nano-CuS) in/on a3 DC u-MOF,[ Cu 3 (BTC) 2 ·(H 2 O) 3 ]( BTC = 1,3,5-benzenetricarboxylate). As the amount of nano-CuS increases in the composite,the electrical conductivity increases exponentially by up to circa 10 9 -fold, while porosity decreases, compared with that of the pristine Cu-MOF.T he composites, nano-CuS(x wt %)@Cu-BTC,exhibit significantly higher electrocatalytic ORR activities than Cu-BTC or nano-CuS in an alkaline solution. The onset potential, electron transfer number,and kinetic current density increase when the electrical conductivity of the material increases but decrease when the material has apoor porosity,which shows that the two factors should be finely tuned by the amount of nano-CuS for ORR application. Of these materials,C uS(28 wt %)@Cu-BTC exhibits the best activity,s howing the onset potential of 0.91 Vv s. RHE, quasi-four-electron transfer pathway,a nd ak inetic current density of 11.3 mA cm À2 at 0.55 Vv s. RHE.Scheme 1. Synthesis of nano-CuS(x wt %)@Cu-BTCand nano-CuS-(99 wt %).Supportinginformation and the ORCID identification number(s) for the author(s) of this article can be found under: http://dx.