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- ItemInfluence of MoS2 on activity and stability of carbon nitride in photocatalytic hydrogen production(Basel : MDPI AG, 2019) Sivasankaran, R.P.; Rockstroh, N.; Kreyenschulte, C.R.; Bartling, S.; Lund, H.; Acharjya, A.; Junge, H.; Thomas, A.; Brückner, A.MoS2/C3N4 (MS-CN) composite photocatalysts have been synthesized by three different methods, i.e., in situ-photodeposition, sonochemical, and thermal decomposition. The crystal structure, optical properties, chemical composition, microstructure, and electron transfer properties were investigated by X-ray diffraction, UV-vis diffuse reflectance spectroyscopy, X-ray photoelectron spectroscopy, electron microscopy, photoluminescence, and in situ electron paramagnetic resonance spectroscopy. During photodeposition, the 2H MoS2 phase was formed upon reduction of [MoS4]2− by photogenerated conduction band electrons and then deposited on the surface of CN. A thin crystalline layer of 2H MoS2 formed an intimate interfacial contact with CN that favors charge separation and enhances the photocatalytic activity. The 2H MS-CN phase showed the highest photocatalytic H2 evolution rate (2342 µmol h−1 g−1, 25 mg catalyst/reaction) under UV-vis light irradiation in the presence of lactic acid as sacrificial reagent and Pt as cocatalyst.
- ItemIn situ powder X-ray diffraction during hydrogen reduction of MoO3 to MoO2(Amsterdam [u.a.] : Elsevier Science, 2022) Burgstaller, M.; Lund, H.; O'Sullivan, M.; Huppertz, H.The hydrogen reduction of molybdenum trioxide to molybdenum dioxide is not yet fully understood as evident by continuous scientific interest. Especially the effect of the potassium content on the reduction process has not yet been considered. We prepared several samples of molybdenum trioxide containing varying amounts of potassium by addition of potassium molybdate (K2MoO4). In situ powder X-ray diffraction experiments were then conducted to study the hydrogen reduction of these samples. We especially focused on the influence of the alkali content and on gaining insight into the importance of the intermediary product γ-Mo4O11. During the reduction process, MoO2 is formed from the reduction of MoO3, which then reacts with the starting material to form γ-Mo4O11. With increasing potassium content, the reduction rate is decreased and the fractional content of γ-Mo4O11 built up during the reduction process is increased. As evident from bulk sample reduction, this results in a significant increase in the grain size visualized via scanning electron microscopy. Our investigations once again underline the importance of γ-Mo4O11 on the morphology of the resulting MoO2 powder.