2D metal coordination polymers have emerged as a new serious of efficient electrocatalysts in OER for their abundant unsaturated coordination centers and high charge-carrier mobility. However, the synthetic routes are mostly depending on the top-down exfoliation with unavoidable structural fragmentation and the annoying sheets’ re-stacking. Here, an electrocatalytic poly (triazine imide) ligand is firstly synthesized and successfully applied to construct the 2D Ni/Fe coordination polymers nanosheets (Ni/Fe-CPNs) through a bottom-up strategy. Average thickness of the nanosheets is around 5 nm, enabling the highly exposed reactive centers. Further benefiting from the ligand promotion effect, absorption of the oxygen species during the OER is effectively accelerated, thus improving the reaction kinetics. Accordingly, the Ni/Fe-CPNs reveals an adorable overpotential of 244 mV at the current density of 10 mA cm⁻², and the Tafel value of 65.8 mv dec⁻¹. Both values are much better than that of commercial RuO₂, and competitive to most of the reported catalysts. The ex-situ techniques, including Raman, FT-IR and XPS analysis alongside with applied potential, are also applied to elaborate the catalytic mechanism. This work offers a new point of view to improve the catalysts’ activity.

二维金属配位聚合物因其丰富的不饱和配位中心和高电荷载流子迁移率而成为 OER 中一类新的高效电催化剂。然而，合成路线主要取决于自上而下的剥离，不可避免的结构破碎和恼人的片材重新堆叠。在这里，首次合成了一种电催化聚（三嗪酰亚胺）配体，并通过自下而上的策略成功应用于构建二维 Ni/Fe 配位聚合物纳米片（Ni/Fe-CPNs）。纳米片的平均厚度约为 5 nm，使高度暴露的反应中心成为可能。进一步受益于配体促进作用，有效加速了 OER 过程中氧物质的吸收，从而改善了反应动力学。因此，^-2，以及 65.8 mv dec ^-1的 Tafel 值。这两个值都比商业 RuO ₂好得多，并且与大多数报道的催化剂相比具有竞争力。非原位技术，包括拉曼、FT-IR 和 XPS 分析以及应用电位，也被用于阐述催化机制。这项工作为提高催化剂的活性提供了新的视角。