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Monitoring the hydrothermal growth of cobalt spinel water oxidation catalysts - From preparative history to catalytic activity

DOI: 10.1002/chem.201801565 DOI Help

Authors: Lukas Reith (University of Zurich) , Karla Lienau (University of Zurich) , Daniel S. Cook (University of Warwick) , Rene More (University of Zurich) , Richard I. Walton (University of Warwick) , Greta Ricarda Patzke (University of Zurich)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Chemistry - A European Journal

State: Published (Approved)
Published: May 2018
Diamond Proposal Number(s): 12884

Abstract: The hydrothermal growth of cobalt oxide spinel (Co₃O₄) nanocrystals from cobalt acetate precursors was monitored with in situ powder X‐ray diffraction (PXRD) in combination with ex situ electron microscopy and vibrational spectroscopy. Kinetic data from in situ PXRD monitoring were analyzed using Sharp‐Hancock and Gualtieri approaches, which both clearly indicate a change of the growth mechanism for reaction temperatures above 185°C. This mechanistic transition goes hand in hand with morphology changes that notably influence the photocatalytic oxygen evolution activity. Complementary quenching investigations of conventional hydrothermal Co₃O₄ growth demonstrate that these insights derived from in situ PXRD data provide valuable synthetic guidelines for water oxidation catalyst production. Furthermore, the ex situ analyses of hydrothermal quenching experiments were essential to assess the influence of amorphous cobalt‐containing phases arising from the acetate precursor on the catalytic activity. Thereby, we illustrate how the efficient combination of a single in situ technique with ex situ analyses paves the way to optimize parameter‐sensitive hydrothermal production processes of key energy materials.

Journal Keywords: In situ monitoring; hydrothermal; nanoparticle; formation mechanisms; photocatalysis; cobalt oxide; water oxidation

Subject Areas: Chemistry, Energy


Instruments: I12-JEEP: Joint Engineering, Environmental and Processing

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