Guiding the directional and effective migration of photocarriers is a basic strategy to achieve high performance of catalysts in the photocatalytic water splitting process.
Guiding the directional and effective migration of photocarriers is a basic strategy to achieve high performance of catalysts in the photocatalytic water splitting process. In this paper, a new carbon material of graphdiyne (GDY) was prepared by a mechanical ball milling method, and then it was introduced into metal oxide Co 3O 4 by an ultrasonic in situ stirring method. The lamellar film structure of GDY provides effective support for Co 3O 4 nanoneedles. It is undeniable that the Co 3O 4/GDY composite has excellent photocatalytic performance for hydrogen production. The highest hydrogen production activity of Co 3O 4/GDY-20 is 2456 μmol g −1, which is 7.7 times that of pure Co 3O 4. In addition, the successful construction of the two-phase S-scheme heterojunction creates favorable conditions for photoelectron migration, and separates the photoelectron–hole pairs successfully. Ultraviolet diffuse reflectance spectra reflect the light absorption capacity of the composite in a wide light wavelength range. Fluorescence spectra and electrochemical detection confirm that photoelectron migration in the composite is effectively regulated, which is very conducive to photocatalytic water splitting. The study shows that the introduction of carbon materials into metal oxides has great potential in the field of photocatalysis.