A novel solution plasma process was developed to assemble honeycomb-like Co–B amorphous alloy catalysts with 253.33 m2 g−1 specific surface area using triethanolamine (TEA) as a soft template. The sample was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron microscopy. During catalytic hydrolysis of hydrous hydrazine (H2NNH2) for hydrogen generation, the hydrolysis activity and hydrogen selectivity of the honeycomb-like Co–B is superior to Rh nanoparticles and Co–B nanospheres. Meanwhile, the sample also exhibits excellent catalytic performance in the catalytic hydrolysis of ammonia borane (NH3BH3) and sodium borohydride (NaBH4) for hydrogen generation, respectively. The H2 generation rate of 28.9, 105.8, and 262.8 L h−1 g−1catalyst for the hydrolysis reactions of H2NNH2, NH3BH3 and NaBH4, respectively, can be achieved. Meanwhile, the honeycomb-like Co–B is found to be a highly stable catalyst as it provides 18 360, 54 000, and 93 727 total turnovers in the hydrolytic dehydrogenations of H2NNH2, NH3BH3 and NaBH4, respectively, after being tested for 30 h. The enhanced catalytic performance for the honeycomb-like Co–B catalyst is attributed to the high specific surface area and the enhanced intrinsic activity resulting from its unique honeycomb-like structure.
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