Rational synthesis of Co-ZIF-67 metal–organic framework (MOF)-derived carbon-supported metal nanoparticles is essential for various energy and environmental applications; however, their catalytic activity toward carbon monoxide (CO) oxidation in various electrolytes is not yet emphasized. Co-ZIF-67-derived hierarchical porous carbon nanosheet-supported Pd nanocrystals (Pd/ZIF-67/C) were prepared using a simple microwave-irradiation approach followed by carbonization and etching. Mechanistically, during microwave irradiation, triethyleneamine provides abundant reducing gases that promote the formation of Pd nanoparticles/Co-Nx in porous carbon nanosheets with the assistance of ethylene glycol and also form a multimodal pore size. The electrocatalytic CO oxidation activity and stability of Pd/ZIF-67/C outperformed those of commercial Pd/C and Pt/C catalysts by (4.2 and 4.4, 4.0 and 2.7, 3.59 and 2.7) times in 0.1 M HClO4, 0.1 M KOH, and 0.1 M NaHCO3, respectively, due to the catalytic properties of Pd besides the conductivity of Co-Nx active sites and delicate porous structures of ZIF-67. Notably, using Pd/ZIF-67/C results in a higher CO oxidation activity than Pd/C and Pt/C. This study may pave the way for using MOF-supported multi-metallic nanoparticles for CO oxidation electrocatalysis.

Metal nanocrystals ornamented metal-organic framework (MOF) are of particular interest in multidisciplinary applications; however, their electrocatalytic CO oxidation performance over wide pH ranges is not yet reported. Herein, Ni-MOF-derived hierarchical...

Nicked-based metal−organic framework-derived carbon (Ni/MOFDC) and its acid-treated counterpart (AT-Ni/ MOFDC) have been prepared as supports for palladium nanoparticle electrocatalysts (Pd/Ni/MOFDC and Pd/AT-Ni/MOFDC). These materials have been prepared using facile microwave-assisted techniques. Several spectroscopic and microscopic techniques (such as FTIR, Raman, PXRD, XPS, XANES, FT-EXAFS, and TEM) have been used to thoroughly characterize physicochemical properties of the materials. It is revealed that acid treatment successfully cleaned the metallic Ni surface of the passivating hydroxides (Ni(OH) 2 and NiOOH) to generate a very low concentration of Ni nanoparticles on the carbon support. The Ni-deficient Pd/AT-Ni/MOFDC shows excellent electrocatalytic performance toward ethanol oxidation reaction (EOR) in the alkaline medium compared to the Ni-hydroxide-rich Pd/Ni/MOFDC counterpart.As a proof-of-concept, these electrocatalysts have been employed as anodes and demonstrated for membraneless direct ethanol microfuel cells (μ-DEFCs) with a micro-3D-printed cell, with FeCo/C as electrocatalyst for the oxygen reduction reaction at the cathode. The Pd/AT-Ni/MOFDC displays increased peak power density (P m = 26.49 mW cm −2 ) with 68% voltage retention after a 24 h galvanostatic discharge test at 40 mA cm −2 and reduced impedance. The improved electrocatalytic properties of the Pd/AT-Ni/MOFDC underscore the need to clean the nickel surface of its passivating hydroxides to harness its full promotional activities toward alcohol oxidation reaction on precious metal electrocatalysts.

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