Oxygen vacancy manipulation and hierarchical morphology construction in oxygen-containing semiconductors have been demonstrated to be effective strategies for developing high efficiency photocatalysts. In most studies of bismuth-based photocatalysts, hierarchical morphology and crystal defects are achieved separately, so the catalysts are not able to benefit from both features. Herein, using boiling ethylene glycol as the treatment solution, we developed an etching-recrystallization method for the fabrication of 3D hierarchical defective BiOCl at ambient pressure. The target hierarchical 3D-BiOCl is composed of self-assembled BiOCl nanosheets, which exhibit a hexagonal prism-like morphology on a micron scale, while simultaneously containing numerous oxygen vacancies within the crystal structure. Consequently, the target catalyst was endowed with a higher specific surface area, greater light harvesting capability, as well as more efficient separation and transfer of photo-excited charges than pristine BiOCl. As a result, 3D-BiOCl presented an impressive photocatalytic activity for the degradation of tetracycline hydrochloride in both visible light and natural white light emitting diode (LED) irradiation. Moreover, an extraordinary recycling property was demonstrated for the target photocatalyst thanks to its hierarchical structure. This study outlines a simple and energy-efficient approach for producing high-performance hierarchically defective BiOCl, which may also open up new possibilities for the morphological and crystal structural defect regulation of other Bi-based photocatalysts.

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