In this study, a series of Ni/Ti bimetallic MOF-derived materials (Sx-NT) were synthesized using a solvothermal sulfur-mediated strategy. The influence of varying thioacetamide dosages on the structural characteristics and photocatalytic hydrogen evolution performance of the materials was systematically investigated. It was found that increasing the thioacetamide content led to a progressive amorphization of the MOF framework, along with the partial formation of nickel sulfide species. Although the original rod-like morphology was largely retained after sulfurization, the surfaces exhibited increased roughness and partial fragmentation, which promoted the exposure of additional active sites. These structural modifications contributed to suppressed recombination of photogenerated charge carriers and improved charge transfer efficiency. The optimized sample, S60-NT, exhibited a hydrogen evolution rate of 1551.98 μmol g −1 ·h −1 , about 5.7 times higher than that of the pristine Ni/Ti MOF. This approach provides a promising strategy for developing high-performance materials for solar-driven hydrogen production and related photocatalytic applications. • Ni/Ti bimetallic MOF-derived materials (Sx-NT) were synthesized via a solvothermal sulfur-mediated strategy. • Sulfur-mediated framework amorphization and surface roughening exposed more active sites for photocatalysis. • The optimized S60-NT sample significantly reduced charge recombination and increased charge transfer efficiency. • S60-NT achieved a hydrogen evolution rate of 1551.98 μmol g −1 h −1 , 5.7 times higher than the pristine Ni/Ti MOF.
Rau et al. (2026) studied this question.