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Open AccessArticle

Structure of Nanocrystalline, Partially Disordered MoS2+δ Derived from HRTEM—An Abundant Material for Efficient HER Catalysis

Institute of Materials Physics, University of Göttingen, Friedrich-Hund-Platz 1, 37077 Göttingen, Germany
Institute for Inorganic and Analytical Chemistry and Freiburg Material Research Center (FMF), University of Freiburg, Albertstraße 21, 79104 Freiburg, Germany
GZG Crystallography University of Göttingen, Goldschmidtstr. 1, 37077 Göttingen, Germany
International Center for Advanced Studies of Energy Conversion (ICASEC), University of Göttingen, D-37077 Göttingen, Germany
Authors to whom correspondence should be addressed.
Catalysts 2020, 10(8), 856;
Received: 5 June 2020 / Revised: 23 July 2020 / Accepted: 28 July 2020 / Published: 1 August 2020
(This article belongs to the Section Electrocatalysis)
Molybdenum sulfides (MoSx, x > 2) are promising catalysts for the hydrogen evolution reaction (HER) that show high hydrogen evolution rates and potentially represent an abundant alternative to platinum. However, a complete understanding of the structure of the most active variants is still lacking. Nanocrystalline MoS2+δ was prepared by a solvothermal method and immobilized on graphene. The obtained electrodes exhibit stable HER current densities of 3 mA cm−2 at an overpotential of ~200 mV for at least 7 h. A structural analysis of the material by high-resolution transmission electron microscopy (HRTEM) show partially disordered nanocrystals of a size between 5–10 nm. Both X-ray and electron diffraction reveal large fluctuations in lattice spacing, where the average c-axis stacking is increased and the in-plane lattice parameter is locally reduced in comparison to the layered structure of crystalline MoS2. A three-dimensional structural model of MoS2+δ could be derived from the experiments, in which [Mo2S12]2− and [Mo3S13]2− clusters as well as disclinations represent the typical defects in the ideal MoS2 structure. It is suggested that the partially disordered nanostructure leads to a high density of coordinatively modified Mo sites with lower Mo–Mo distances representing the active sites for HER catalysis, and, that these structural features are more important than the S:Mo ratio for the activity. View Full-Text
Keywords: hydrogen evolution catalysis; molybdenum sulfides; nanocrystalline materials hydrogen evolution catalysis; molybdenum sulfides; nanocrystalline materials
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Ronge, E.; Hildebrandt, S.; Grutza, M.-L.; Klein, H.; Kurz, P.; Jooss, C. Structure of Nanocrystalline, Partially Disordered MoS2+δ Derived from HRTEM—An Abundant Material for Efficient HER Catalysis. Catalysts 2020, 10, 856.

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