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Designing highly active and durable electrocatalysts remain an ongoing challenge in the oxygen reduction reaction (ORR). Here, the reductive IL/Ti3C2Tx(FA) is produced in a water‐free mixture of formic acid (FA), ionic liquid (IL) and LiF, subsequently, the simultaneous reduction encapsulation trap the Pd nanocatalysts and IL within bilayer carbide‐derived carbon (CDC) to obtain Pd@IL/CDC(FA) with high metal loading up to 69.7%. Thereby, the featured active phases in Pd@IL/CDC(FA) impart potent chemical nanoconfinement to defend metals from dissolution and aggregation, boost mass and electron transfer, and mediate oxidation states and adsorption/desorption of metal Pd in the ORR. Instead of deactivation and Ostwald ripening, the catalytic performances of Pd@IL/CDC(FA) are gradually enhanced in an accelerated durability test up to 20 000 cycles. In a Zn–air battery, the Pd@IL/CDC(FA) cathode gives a specific capacity of 812.6 mAh gZn−1 and a voltage loss of only 41 mV in galvanostatic discharge for 1000 h. The work opens new venues in controllably preparing high activity and durable electrocatalysts from in‐situ generated CDCs. [ABSTRACT FROM AUTHOR]

The charge transfer and active sites of metal-free imidazolium-based composites were unveiled by an electrochemical method with high sensitivity and selectivity due to the specific donor–acceptor coupling of imidazolium with NO2−. [ABSTRACT FROM AUTHOR]