biostudies-literatureHarouna-Mayer SYEuropean Research CouncilDeutsche Forschungsgemeinschaft (DFG), Cluster of Excellence "Advanced Imaging of Matter"Bundesministerium für Bildung und Forschung, Erforschung von Universum und Materie (ErUM)e2506838https://www.ebi.ac.uk/biostudies/studies/S-EPMC12372454biostudies-literatureUnknown21(33)Transition metal nitrides (TMNs) are emerging as a promising class of materials for application in optoelectronics as well as energy conversion and storage, but they remain rather unexplored, mainly due to a lack of mechanistic understanding of their synthetic pathways. Here, a one-pot synthesis is demonstrated, which yields 3 nm phase-pure Cu<sub>3</sub>PdN nanoparticles after the reaction of Cu methoxide and Pd acetylacetonate in benzylamine for 5 min at 140 °C. The structure of the initial complexes and their conversion to Cu<sub>3</sub>PdN are revealed by in situ X-ray absorption spectroscopy measurements and elucidate nucleation and growth of the nitride nanocrystals by in situ total X-ray scattering measurements. Interestingly, extended X-ray absorption fine structure double-edge refinement reveals the presence of short-range cation-site disorder in the anti-perovskite structure of Cu<sub>3</sub>PdN, which has not been observed before in the Cu<sub>3</sub>PdN system. Additionally, the synthesized Cu<sub>3</sub>PdN nanoparticles are tested for the electrocatalytic hydrogen evolution reaction, revealing an overpotential as low as η<sub>10</sub> = 212 ± 11 mV measured at 10 mA cm<sup>-2</sup>.Small (Weinheim an der Bergstrasse, Germany)Cation-Site Disordered Cu<sub>3</sub>PdN Nanoparticles for Hydrogen Evolution Electrocatalysis.PMC1237245439071599481894105K22GU7 (LUCENT II)EXC2056Belgardt LMathon OHsu CSKlemeyer LGroene TRLAkcaalan MGNoei HKoppen AKipping LHarouna-Mayer SYCaddeo FKoziej DKopula Kesavan JDippel ACfalseCation-Site Disordered Cu<sub>3</sub>PdN Nanoparticles for Hydrogen Evolution Electrocatalysis.Transition metal nitrides (TMNs) are emerging as a promising class of materials for application in optoelectronics as well as energy conversion and storage, but they remain rather unexplored, mainly due to a lack of mechanistic understanding of their synthetic pathways. Here, a one-pot synthesis is demonstrated, which yields 3 nm phase-pure Cu<sub>3</sub>PdN nanoparticles after the reaction of Cu methoxide and Pd acetylacetonate in benzylamine for 5 min at 140 °C. The structure of the initial complexes and their conversion to Cu<sub>3</sub>PdN are revealed by in situ X-ray absorption spectroscopy measurements and elucidate nucleation and growth of the nitride nanocrystals by in situ total X-ray scattering measurements. Interestingly, extended X-ray absorption fine structure double-edge refinement reveals the presence of short-range cation-site disorder in the anti-perovskite structure of Cu<sub>3</sub>PdN, which has not been observed before in the Cu<sub>3</sub>PdN system. Additionally, the synthesized Cu<sub>3</sub>PdN nanoparticles are tested for the electrocatalytic hydrogen evolution reaction, revealing an overpotential as low as η<sub>10</sub> = 212 ± 11 mV measured at 10 mA cm<sup>-2</sup>.2025-01-01T00:00:00Z2025 Aug2026-05-09T10:35:16.128Z2026-04-08T00:47:02.58ZS-EPMC123724544053823710.1002/smll.202506838