Herein, in order to promote the scaled-up manufacturing of efficient nanostructured electrocatalysts, we pioneer a novel ultrafast wet chemistry engineering to turn bulk Co-Ni foam into S activated hydroxide based nanosheets (CoNi-OH|S), with short period less than six minutes. The uniform nanosheets morphology is in-situ formed through designed nitro-hydrochloric acid enhanced corrosion within 30 s, then the nanosheets are naturally oxidized to CoOOH/Ni(OH)₂ (CoNi-OH) when drying in the air. To fully boost the electrochemical activities, S activation is conducted through facile chemical bath in S anion-rich aqueous solution with five minutes. The as formed surface sulfur species could optimize the protons adsorption, thus benefitting the HER electrocatalysis. Besides, the Co³⁺ sites with low coordination are also increased by S activation, which could facilitate the de-protonation of OOH, thus promoting the OER electrocatalysis. Finally, such ultrafast surface engineering derived CoNi-OH|S electrodes afford the relatively low overpotentials of 167 mV for HER and 270 mV for OER at 10 mA cm⁻². This wet chemistry strategy further ensures that the large area self-supported electrodes can be easily prepared within several minutes, which would inspire the large-scale synthesis and practical application of similar electrocatalysts in this field.

在此，为了促进大规模生产高效的纳米结构电催化剂，我们率先提出了一种新颖的超快湿化学工程技术，可将短时间内的Co-Ni泡沫材料转变为S活化氢氧化物基纳米片（CoNi-OH | S）。六分钟 通过设计的硝基盐酸增强腐蚀在30 s内原位形成均匀的纳米片形态，然后在空气中干燥时，纳米片自然氧化为CoOOH / Ni（OH）₂（CoNi-OH）。为了充分增强电化学活性，在富含S阴离子的水溶液中通过五分钟的便捷化学浴进行S活化。所形成的表面硫物质可以优化质子吸附，从而有利于HER电催化。此外，Co ³⁺S活化也增加了低配位的位点，这可以促进OOH的去质子化，从而促进OER电催化。最后，这种超快速表面工程衍生的CoNi-OH | S电极在10 mA cm ^-2时具有相对较低的过电势，HER为167 mV，OER为270 mV 。这种湿化学策略进一步确保了大面积自支撑电极可以在几分钟之内轻松制备，这将激发类似电催化剂在该领域的大规模合成和实际应用。