Electrocatalytic conversion of nitrite (NO₂⁻) to ammonia (NH₃) via the NO₂⁻ reduction reaction (eNO₂RR) presents a promising approach. Prussian blue analog (PBA)–based electrocatalysts are potential candidates for eNO₂RR owing to their good activity and selectivity. Herein, to the best of our knowledge, for the first time, we report a facile synthesis of a flower-like copper (Cu)–cobalt (Co) PBA sulfide (CuCoPBA-S) using pulsed laser irradiation in liquid and investigate its formation mechanism using acoustic levitation coupled with in situ Raman spectroscopy. This approach enables contaminant-free, rapid, and cost-effective synthesis of electrocatalysts. The sulfurization process is shown to be time-dependent in the formation of ordered/disordered flower-like CuCoPBA-S structures. CuCoPBA-S considerably influences the eNO₂RR, achieving a NH₃ faradaic efficiency (FE) of 80.91% and an NH₃ yield rate of 3394.1 μg h⁻¹ cm⁻² at a fixed potential of −0.5 V vs. the reversible hydrogen electrode (RHE). Moreover, density functional theory analysis validates the eNO₂RR pathway facilitated by CuCoPBA-S during the electrocatalytic conversion of NO₂⁻ to NH₃, and the rate-determining step in the pathway is the hydrogenation of *NH₂O to *NH₂OH.

Here, furfural oxidation was performed to replace the kinetically sluggish O₂ evolution reaction (OER). Pt-Co₃O₄ nanospheres were developed via pulsed laser ablation in liquid (PLAL) in a single step for the paired electrocatalysis of an H₂ evolution reaction (HER) and furfural oxidation reaction (FOR). The FOR afforded a high furfural conversion (44.2%) with a major product of 2-furoic acid after a 2-h electrolysis at 1.55 V versus reversible hydrogen electrode in a 1.0-M KOH/50-mM furfural electrolyte. The Pt-Co₃O₄ electrode exhibited a small overpotential of 290 mV at 10 mA cm⁻². As an anode and cathode in an electrolyzer system, the Pt-Co₃O₄ electrocatalyst required only a small applied cell voltage of ~1.83 V to deliver 10 mA cm⁻², compared with that of the pure water electrolyzer (OER||HER, ~1.99 V). This study simultaneously realized the integrated production of energy-saving H₂ fuel at the cathode and 2-furoic acid at the anode.