Hydrogen production via electrocatalytic reduction of water is a promising clean-energy technology. For further advancement of this technology, the exploration of cost-effective and streamlined approaches for producing active phosphide-based catalysts is of great importance. This study presents a new high-temperature preparation method of a microporous Ni₂P/C catalyst composed of crystalline Ni₂P nanoparticles homogeneously distributed within an amorphous carbon matrix in a weight ratio of 40/60. The redox transformation leading to the formation of Ni₂P from not-reduced stable inorganic salts was facilitated during thermal treatment by a polymeric precursor, which, in turn, transformed into microporous carbon matrix that prevented the newly formed phosphide particles from agglomerating and sintering. The microporous structure of the prepared composite was characterised by gas adsorption technique and modelled using density functional theory and statistical thickness methods. The t-plot revealed high micropore surface area of 333.5 m² g⁻¹ (accounting 97 % of total surface area) and the pore size distribution in the range of 10–12 Å. According to TEM analysis, the size range of the Ni₂P inclusions varied from 5 to 200 nm. The evaluation of electrocatalytic properties of the Ni₂P/C composite demonstrated its high HER activity and stability under high voltages in alkaline water electrolysis conditions. Furthermore, HER activity of the composite was substantially enhanced by grinding, which opened closed microporosity channels and increased the micropore surface area to 355.2 m² g⁻¹, thereby increasing the number of catalytically active sites in the sample. The result indicates the exceptional role of the microporous microstructure of the composite in its catalytic performance. The findings of this study may have a significant impact on the practical implementation of efficient hydrogen production by water electrolysis.

通过电催化还原水制氢是一种很有前途的清洁能源技术。为了进一步推进这项技术，探索具有成本效益和简化的生产活性磷化物基催化剂的方法非常重要。本研究提出了一种新的高温制备微孔Ni ₂ P/C催化剂的方法，该催化剂由结晶Ni ₂ P纳米颗粒以40/60的重量比均匀分布在无定形碳基体中组成。在热处理过程中，聚合前体促进了未还原的稳定无机盐形成 Ni 2 P 的氧化还原转化，进而转化为微孔碳基质，防止新形成的磷化物颗粒团聚和烧结_。通过气体吸附技术对所制备的复合材料的微孔结构进行了表征，并使用密度泛函理论和统计厚度方法进行了建模。t 图显示微孔表面积高达 333.5 m ²  g ^-1（占总表面积的 97%），孔径分布在 10–12 Å 范围内。根据TEM分析，Ni ₂ P夹杂物的尺寸范围为5至200 nm。_{Ni 2} P/C复合材料的电催化性能评估表明其在碱性水电解条件下高电压下具有较高的HER活性和稳定性。此外，复合材料的HER活性通过研磨得到显着增强，打开了封闭的微孔通道并将微孔表面积增加至355.2 m ²  g ^-1，从而增加了样品中催化活性位点的数量。结果表明复合材料的微孔微观结构对其催化性能的特殊作用。这项研究的结果可能对水电解高效制氢的实际实施产生重大影响。