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Title: Non-Equilibrium Synthesis of Highly Active Nanostructured, Oxygen-Incorporated Amorphous Molybdenum Sulfide HER Electrocatalyst

Abstract

Abstract Molybdenum sulfide emerged as promising hydrogen evolution reaction (HER) electrocatalyst thanks to its high intrinsic activity, however its limited active sites exposure and low conductivity hamper its performance. To address these drawbacks, the non‐equilibrium nature of pulsed laser deposition (PLD) is exploited to synthesize self‐supported hierarchical nanoarchitectures by gas phase nucleation and sequential attachment of defective molybdenum sulfide clusters. The physics of the process are studied by in situ diagnostics and correlated to the properties of the resulting electrocatalyst. The as‐synthesized architectures have a disordered nanocrystalline structure, with nanodomains of bent, defective S‐Mo‐S layers embedded in an amorphous matrix, with excess sulfur and segregated molybdenum particles. Oxygen incorporation in this structure fosters the creation of amorphous oxide/oxysulfide nanophases with high electrical conductivity, enabling fast electron transfer to the active sites. The combined effect of the nanocrystalline pristine structure and the surface oxidation enhances the performance leading to small overpotentials, very fast kinetics (35.1 mV dec −1 Tafel slope) and remarkable long‐term stability for continuous operation up to ‐1 A cm −2 . This work shows possible new avenues in catalytic design arising from a non‐equilibrium technique as PLD and the importance of structural and chemical control to improve themore » HER performance of MoS‐based catalysts.« less

Authors:
 [1];  [2];  [1];  [2];  [3];  [2]; ORCiD logo [4];  [5]; ORCiD logo [4]; ORCiD logo [4];  [3];  [6];  [6];  [5]; ORCiD logo [4]; ORCiD logo [4]; ORCiD logo [2]
+ Show Author Affiliations
  1. Inst. Italiano di Tecnologia, Milan (Italy); Politecnico di Milano, Milan (Italy)
  2. Inst. Italiano di Tecnologia, Milan (Italy)
  3. Inst. Italiano di Tecnologia, Genova (Italy)
  4. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)
  5. Univ. of Tennessee, Knoxville, TN (United States)
  6. Univ. of Cambridge (United Kingdom)
Publication Date:
Research Org.:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Science & Engineering Division; USDOE
OSTI Identifier:
1766414
Alternate Identifier(s):
OSTI ID: 1804822
Grant/Contract Number:  
AC05-00OR22725
Resource Type:
Accepted Manuscript
Journal Name:
Small
Additional Journal Information:
Journal Volume: 16; Journal Issue: 44; Journal ID: ISSN 1613-6810
Publisher:
Wiley
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; a-MoSx; electrocatalysis; hydrogen evolution reaction; non-equilibrium synthesis; pulsed laser deposition

Citation Formats

Giuffredi, Giorgio, Mezzetti, Alessandro, Perego, Andrea, Mazzolini, Piero, Prato, Mirko, Fumagalli, Francesco, Lin, Yu‐Chuan, Liu, Chenze, Ivanov, Ilia N., Belianinov, Alex, Colombo, Massimo, Divitini, Giorgio, Ducati, Caterina, Duscher, Gerd, Puretzky, Alexander A., Geohegan, David B., and Di Fonzo, Fabio. Non-Equilibrium Synthesis of Highly Active Nanostructured, Oxygen-Incorporated Amorphous Molybdenum Sulfide HER Electrocatalyst. United States: N. p., 2020. Web. doi:10.1002/smll.202004047.
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Giuffredi, Giorgio, Mezzetti, Alessandro, Perego, Andrea, Mazzolini, Piero, Prato, Mirko, Fumagalli, Francesco, Lin, Yu‐Chuan, Liu, Chenze, Ivanov, Ilia N., Belianinov, Alex, Colombo, Massimo, Divitini, Giorgio, Ducati, Caterina, Duscher, Gerd, Puretzky, Alexander A., Geohegan, David B., & Di Fonzo, Fabio. Non-Equilibrium Synthesis of Highly Active Nanostructured, Oxygen-Incorporated Amorphous Molybdenum Sulfide HER Electrocatalyst. United States. https://doi.org/10.1002/smll.202004047
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Giuffredi, Giorgio, Mezzetti, Alessandro, Perego, Andrea, Mazzolini, Piero, Prato, Mirko, Fumagalli, Francesco, Lin, Yu‐Chuan, Liu, Chenze, Ivanov, Ilia N., Belianinov, Alex, Colombo, Massimo, Divitini, Giorgio, Ducati, Caterina, Duscher, Gerd, Puretzky, Alexander A., Geohegan, David B., and Di Fonzo, Fabio. Thu . "Non-Equilibrium Synthesis of Highly Active Nanostructured, Oxygen-Incorporated Amorphous Molybdenum Sulfide HER Electrocatalyst". United States. https://doi.org/10.1002/smll.202004047. https://www.osti.gov/servlets/purl/1766414.
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@article{osti_1766414,
title = {Non-Equilibrium Synthesis of Highly Active Nanostructured, Oxygen-Incorporated Amorphous Molybdenum Sulfide HER Electrocatalyst},
author = {Giuffredi, Giorgio and Mezzetti, Alessandro and Perego, Andrea and Mazzolini, Piero and Prato, Mirko and Fumagalli, Francesco and Lin, Yu‐Chuan and Liu, Chenze and Ivanov, Ilia N. and Belianinov, Alex and Colombo, Massimo and Divitini, Giorgio and Ducati, Caterina and Duscher, Gerd and Puretzky, Alexander A. and Geohegan, David B. and Di Fonzo, Fabio},
abstractNote = {Abstract Molybdenum sulfide emerged as promising hydrogen evolution reaction (HER) electrocatalyst thanks to its high intrinsic activity, however its limited active sites exposure and low conductivity hamper its performance. To address these drawbacks, the non‐equilibrium nature of pulsed laser deposition (PLD) is exploited to synthesize self‐supported hierarchical nanoarchitectures by gas phase nucleation and sequential attachment of defective molybdenum sulfide clusters. The physics of the process are studied by in situ diagnostics and correlated to the properties of the resulting electrocatalyst. The as‐synthesized architectures have a disordered nanocrystalline structure, with nanodomains of bent, defective S‐Mo‐S layers embedded in an amorphous matrix, with excess sulfur and segregated molybdenum particles. Oxygen incorporation in this structure fosters the creation of amorphous oxide/oxysulfide nanophases with high electrical conductivity, enabling fast electron transfer to the active sites. The combined effect of the nanocrystalline pristine structure and the surface oxidation enhances the performance leading to small overpotentials, very fast kinetics (35.1 mV dec −1 Tafel slope) and remarkable long‐term stability for continuous operation up to ‐1 A cm −2 . This work shows possible new avenues in catalytic design arising from a non‐equilibrium technique as PLD and the importance of structural and chemical control to improve the HER performance of MoS‐based catalysts.},
doi = {10.1002/smll.202004047},
journal = {Small},
number = 44,
volume = 16,
place = {United States},
year = {Thu Oct 08 00:00:00 EDT 2020},
month = {Thu Oct 08 00:00:00 EDT 2020}
}
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Porous MS 2 /MO 2 (M = W, Mo) Nanorods as Efficient Hydrogen Evolution Reaction Catalysts
journal, September 2016

Determination of adsorption of OPD H species in the cathodic hydrogen evolution reaction at Pt in relation to electrocatalysis
journal, January 1986

  • Conway, B. E.; Bai, Lijun
  • Journal of Electroanalytical Chemistry and Interfacial Electrochemistry, Vol. 198, Issue 1
  • DOI: 10.1016/0022-0728(86)90033-1

Dynamics of plume propagation, splitting, and nanoparticle formation during pulsed-laser ablation
journal, May 1998

Use of Platinum as the Counter Electrode to Study the Activity of Nonprecious Metal Catalysts for the Hydrogen Evolution Reaction
journal, April 2017

Identification of Active Edge Sites for Electrochemical H2 Evolution from MoS2 Nanocatalysts
journal, July 2007

  • Jaramillo, T. F.; Jorgensen, K. P.; Bonde, J.
  • Science, Vol. 317, Issue 5834, p. 100-102
  • DOI: 10.1126/science.1141483

Efficient hydrogen evolution by ternary molybdenum sulfoselenide particles on self-standing porous nickel diselenide foam
journal, September 2016

  • Zhou, Haiqing; Yu, Fang; Huang, Yufeng
  • Nature Communications, Vol. 7, Issue 1
  • DOI: 10.1038/ncomms12765

The hydrogen economy in the 21st century: a sustainable development scenario
journal, March 2003

A comprehensive review on PEM water electrolysis
journal, April 2013

  • Carmo, Marcelo; Fritz, David L.; Mergel, Jürgen
  • International Journal of Hydrogen Energy, Vol. 38, Issue 12, p. 4901-4934
  • DOI: 10.1016/j.ijhydene.2013.01.151

Electrochemistry of Nanostructured Layered Transition-Metal Dichalcogenides
journal, October 2015

In situ laser raman spectroscopy of the sulfiding of Mo/$gamma;-Al2O3 catalysts
journal, April 1983

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