ABSTRACT Inspired by the demand to solve the eco‐crisis, designing and engineering‐shaped photocatalysts for industrial liquid‐phase pollutant treatments remains crucial. Here, we designed a novel monolithic BiPO 4 @ mono MIL‐100(Fe) composite fabricated via a one‐pot sol–gel strategy with gradient concentration of BiPO 4 . The characterizations confirm that the introduction of BiPO 4 does not disrupt the crystal structure of mono MIL‐100(Fe), while the composite with 8 wt% loading demonstrates a high specific surface area. Photocatalytic degradation of TCH reveals that the optimized 8 wt% BiPO 4 @ mono MIL‐100 achieves a 94% degradation rate under visible light irradiation, attributable to the interaction between the two composites and the broad‐spectrum response characteristics of the heterojunction. Further, excessive loading leads to reduced degradation efficiency due to BiPO 4 aggregation and consequent decrease in active sites. The BiPO 4 @ mono MIL‐100 also showed great recycle ability and mechanical stability. The radicals capture experiments indicated that holes (h + ) are the primary active species responsible for the photocatalytic degradation of tetracycline. Based on the band structure of the Type‐II heterojunction, photogenerated electrons migrate from mono MIL‐100(Fe) to BiPO 4 , while holes accumulate in the valence band (VB) of mono MIL‐100(Fe) from BiPO 4 and then directly oxidize and decompose tetracycline. This work provides a novel methodology for morphology control and performance optimization of MOF‐based composite catalysts.
Wang et al. (Mon,) studied this question.