This work reports the first preparation and characterization of a hybrid PbS quantum dot (QD)/nanoporous NiO film nanostructure as well as its application for novel self-powered cathodic photoelectrochemical (PEC) sensing. Specifically, we synthesized the thioglycolic acid-capped PbS QDs and then assembled them onto the hydrothermally fabricated three-dimensional (3D) NiO nanostructured films on the transparent indium tin oxide-coated glass substrates, followed by the subsequent conjugation with the glucose oxidase as a model biocatalyst. Favorable alignment existed between the NiO and PbS QDs, and the as-obtained p-type heterostructure was characterized by various techniques and found to have good PEC activities. In the self-powered PEC biosensing of glucose, the system exhibited high sensitivity toward the presence of dissolved oxygen in the electrolyte, and thereby, a novel PEC enzymatic sensor was developed. With a PbS QD/3D NiO nanofilm, this work manifested the great promise of a heterostructure photocathode for a self-powered PEC biosensor that to the best of our knowledge has not been reported. We believe that it could inspire more interest in the design and development of numerous other p-type heterostructures for advanced self-powered PEC biosensors.

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