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In Situ Monitoring of Nanoparticle Formation during Iridium-Catalysed Oxygen Evolution by Real-Time Small Angle X-Ray Scattering

Singer Hobbs, Maya ; Sackville, Emma V. ; Smith, Andrew J. ; Edler, Karen J. LU orcid and Hintermair, Ulrich (2019) In ChemCatChem 11(21). p.5313-5321
Abstract

Real-time Small Angle X-Ray Scattering (SAXS) has been used to investigate the homogeneity of a series of molecular iridium complexes during water oxidation catalysis in aqueous NaIO4 solution through a continuous flow cell. The results obtained for the unstable [Cp*Ir(OH2)3]2+ precursor forming amorphous IrOx nanoparticles (NPs) in-situ validate and complement previous Dynamic Light Scattering (DLS) studies by providing enhanced sensitivity for small particle sizes and increased temporal resolution under realistic reaction conditions. Correlating particle formation profiles with O2 evolution traces allowed homogeneous catalysis to be clearly distinguished from... (More)

Real-time Small Angle X-Ray Scattering (SAXS) has been used to investigate the homogeneity of a series of molecular iridium complexes during water oxidation catalysis in aqueous NaIO4 solution through a continuous flow cell. The results obtained for the unstable [Cp*Ir(OH2)3]2+ precursor forming amorphous IrOx nanoparticles (NPs) in-situ validate and complement previous Dynamic Light Scattering (DLS) studies by providing enhanced sensitivity for small particle sizes and increased temporal resolution under realistic reaction conditions. Correlating particle formation profiles with O2 evolution traces allowed homogeneous catalysis to be clearly distinguished from heterogeneous catalysis. A series of seven pyridine−alkoxide Cp*Ir complexes are shown to be fully homogeneous by SAXS, validating previous studies and confirming their catalysis to be molecular in nature throughout the reaction.

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author
; ; ; and
publishing date
type
Contribution to journal
publication status
published
keywords
homogeneous vs. heterogeneous catalysis, iridium, nanoparticles, SAXS, water oxidation
in
ChemCatChem
volume
11
issue
21
pages
9 pages
publisher
John Wiley & Sons Inc.
external identifiers
  • scopus:85071887575
ISSN
1867-3880
DOI
10.1002/cctc.201901268
language
English
LU publication?
no
additional info
Publisher Copyright: © 2019 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.
id
3116a848-68f1-4d6d-9190-f1ff39dd6ccc
date added to LUP
2023-01-18 09:05:19
date last changed
2023-01-18 14:04:40
@article{3116a848-68f1-4d6d-9190-f1ff39dd6ccc,
  abstract     = {{<p>Real-time Small Angle X-Ray Scattering (SAXS) has been used to investigate the homogeneity of a series of molecular iridium complexes during water oxidation catalysis in aqueous NaIO<sub>4</sub> solution through a continuous flow cell. The results obtained for the unstable [Cp*Ir(OH<sub>2</sub>)<sub>3</sub>]<sup>2+</sup> precursor forming amorphous IrO<sub>x</sub> nanoparticles (NPs) in-situ validate and complement previous Dynamic Light Scattering (DLS) studies by providing enhanced sensitivity for small particle sizes and increased temporal resolution under realistic reaction conditions. Correlating particle formation profiles with O<sub>2</sub> evolution traces allowed homogeneous catalysis to be clearly distinguished from heterogeneous catalysis. A series of seven pyridine−alkoxide Cp*Ir complexes are shown to be fully homogeneous by SAXS, validating previous studies and confirming their catalysis to be molecular in nature throughout the reaction.</p>}},
  author       = {{Singer Hobbs, Maya and Sackville, Emma V. and Smith, Andrew J. and Edler, Karen J. and Hintermair, Ulrich}},
  issn         = {{1867-3880}},
  keywords     = {{homogeneous vs. heterogeneous catalysis; iridium; nanoparticles; SAXS; water oxidation}},
  language     = {{eng}},
  month        = {{11}},
  number       = {{21}},
  pages        = {{5313--5321}},
  publisher    = {{John Wiley & Sons Inc.}},
  series       = {{ChemCatChem}},
  title        = {{In Situ Monitoring of Nanoparticle Formation during Iridium-Catalysed Oxygen Evolution by Real-Time Small Angle X-Ray Scattering}},
  url          = {{http://dx.doi.org/10.1002/cctc.201901268}},
  doi          = {{10.1002/cctc.201901268}},
  volume       = {{11}},
  year         = {{2019}},
}