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A dual-electrode coupling with Pts,n @NiS2 @CC cathode and CuO/CF anode lowers cell voltage to 0.96 V at 10 mA cm−2 and improves energy efficiency, supported by in situ spectroscopy and theory, with stable operation beyond 300 h and industrial-grade current density.",{"@graph":14,"@context":72},[15,34,55],{"@type":16,"itemListElement":17},"BreadcrumbList",[18,23,27,31],{"item":19,"name":20,"@type":21,"position":22},"https://docshare.wps.com","Home","ListItem",1,{"item":24,"name":25,"@type":21,"position":26},"https://docshare.wps.com/document/","Document",2,{"item":28,"name":29,"@type":21,"position":30},"https://docshare.wps.com/document/research-report/","Research & 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[https://doi.org/10.1007/s40820-025-02025-3](https://doi.org/10.1007/s40820-025-02025-3)  \nCite as  \nNano-Micro Lett.(2026) 18:197  \nReceived: 20 August 2025  \nAccepted: 19 November 2025  \nPublished online: 4 January 2026 © The Author(s) 2026  \nElectrocatalytic Self‑Coupling of N‑Heterocyclic Amides for Energy‑Efficient Bipolar Hydrogen Production  \nYuqiang Ma 1, Meng Li 1, Dandan Zhang 1, Cihang Wang 1, Yu Li 1, Zihang Zhao 1, Xiaogang Mu2, Jun Hu 1, Xiang Hu3 *, Jiachen Li 1 *, Haixia Ma 1,2 *, Zhenhai Wen3  \nHIGHLIGHTS  \n• Replacing anodic oxygen evolution reaction with 3,5-diamino-1,2,4-triazole oxidative coupling enables ultra-low-voltage (0.96 V @10 mA cm− 2) dual-electrode H2 production and simultaneous synthesis of energetic 5,5′-diamino-3,3′-azido-1H-1,2,4-triazole (DAAT), achieving 35.8% energy savings.  \n• A Pt single-atom/nanoparticle hybrid on NiS2 nanosheets (Pts,n @NiS2 @CC) exhibits exceptional alkaline hydrogen evolution reaction performance and stability via optimized H* adsorption.  \n• Anodic DAAT formation proceeds via an OH*-mediated N–N coupling pathway, enabling stable (> 300 h @500 mA cm− 2), industrialscale bipolar H2 production coupled with green DAAT synthesis in an anion-exchange membrane water electrolyzer.  \nABSTRACT This study proposes a green electrochemical strategy for addressing the high-energy-barrier oxygen evolution reaction (OER) in traditional overall water splitting. Leveraging the thermodynamic advantages of N–H bond activation/cleavage and N–N coupling processes, the 3,5-diamino-1,2,4-triazole (DAT) oxidative coupling reaction (DATOR) has been introduced to replace the high-energy-barrier oxygen evolution reaction (OER). This substitution enables low-energy-consumption hydrogen production while simultaneously yielding high-value azo energetic materials. Furthermore, to enhance electron and atom economy, the anodic DATOR process allows the hydrogen radicals (H*) generated from amine dehydrogenation to chemically combine via the Tafel process, producing hydrogen gas. By constructing coupling system with Pts,n @NiS2 @CC cathode and CuO/CF anode, the operating voltage of the system was significantly reduced (0.96 V@10 mA cm− 2), which was 680 mV more energy efficient than conventional water electrolysis (1.64 V). In situ spectroscopy and theoretical calculations indicate that the anode DATOR generates DAAT through theN–H bond cleavage and N–N coupling path mediated by hydroxyl radicals (OH*), while releasing hydrogen gas. The coupling system has been operating stably for more than 300 h at an industrial-grade current density. This research provides new ideas for dual-electrode hydrogen production and green electrosynthesis of functional materials, with significant energy and economic benefits.  \nKEYWORDS Bipolar hydrogen production; Electrosynthesis; Coupling system; 5,5′-diamino-3,3′-azo-1H-1,2,4-triazole; Pt-based catalyst  \n* Xiang Hu, [huxiang@fjirsm.ac.cn](huxiang@fjirsm.ac.cn); Jiachen Li, [lijiachen@nwu.edu.cn](lijiachen@nwu.edu.cn); Haixia Ma, [mahx@nwu.edu.cn](mahx@nwu.edu.cn)  \n1 Xi’an Key Laboratory of Special Energetic Materials, School of Chemical Engineering, Northwest University, Xi’an 710127, People’s Republic of China  \n2 Zhijian Laboratory, Xi’an 710025, People’s Republic of China  \n3 State Key Laboratory of Structural Chemistry, and Fujian Provincial Key Laboratory of Materials and Techniques Toward Hydrogen Energy, Fujian Institute of Research On the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, People’s Republic of China  \n1 Introduction  \nHydrogen is considered a promising energy source to replace fossil fuels in the future [1–3] . Among them, hydrogen production by electrolysis of water is an environmentally friendly and efficient means of hydrogen production [4–6] . At present, hydrogen production from water electrolysis has not been applied on a large scale, the fundamental reason being that the s","cbCaimbPJIUgeZpa","https://ap.wps.com/l/cbCaimbPJIUgeZpa","pdf",9428740,"English","# Highlights\n## Abstract\n## Key terms\n# Introduction","[{\"question\":\"What strategy replaces oxygen evolution reaction in this study?\",\"answer\":\"The work replaces the anode oxygen evolution reaction with a DAT oxidative self-coupling route (DATOR), enabling hydrogen production at lower energy while simultaneously generating energetic DAAT materials.\"},{\"question\":\"How does the hydrogen evolution and coupling system achieve energy savings?\",\"answer\":\"A dual-electrode coupling system with a Pts,n @NiS2 @CC cathode and CuO/CF anode reduces the operating voltage to 0.96 V at 10 mA cm−2, reported as 680 mV more energy efficient than conventional electrolysis.\"},{\"question\":\"What evidence supports the mechanism of DAAT formation?\",\"answer\":\"In situ spectroscopy and theoretical calculations indicate that the anode DATOR forms DAAT via an OH*-mediated N–N coupling pathway after N–H bond cleavage.\"}]","Electrocatalytic Self-Coupling of N-Heterocyclic Amides for Energy-Efficient Bipolar Hydrogen Production | PDF",1790686248]