Chemical Insights into the Formation of Colloidal Iridium Nanoparticles from In Situ X-ray Total Scattering: Influence of Precursors and Cations on the Reaction Pathway

Mathiesen, Jette K.; Quinson, Jonathan; Blaseio, Sonja; Kjær, Emil T. S.; Dworzak, Alexandra; Cooper, Susan R.; Pedersen, Jack K.; Wang, Baiyu; Bizzotto, Francesco; Schröder, Johanna; Kinnibrugh, Tiffany L.; Simonsen, Søren B.; Theil Kuhn, Luise; Kirkensgaard, Jacob J. K.; Rossmeisl, Jan; Oezaslan, Mehtap; Arenz, Matthias; Jensen, Kirsten M. Ø.

doi:10.1021/jacs.2c10814

Chemical Insights into the Formation of Colloidal Iridium Nanoparticles from In Situ X-ray Total Scattering: Influence of Precursors and Cations on the Reaction Pathway

Journal Article · Tue Jan 10 23:00:00 EST 2023 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.2c10814· OSTI ID:2000031

Mathiesen, Jette K. ^[1]; ^[2]; ^[3]; Kjær, Emil T. S. ^[4]; ^[3]; Cooper, Susan R. ^[4]; ^[4]; Wang, Baiyu ^[4]; Bizzotto, Francesco ^[5]; ^[5]; Kinnibrugh, Tiffany L. ^[6]; ^[7]; Theil Kuhn, Luise ^[7]; ^[4]; ^[4]; ^[3]; ^[5]; ^[4]

University of Copenhagen (Denmark); Technical University of Denmark, Lyngby (Denmark)
University of Copenhagen (Denmark); Aarhus University (Denmark)
Technische Universität Braunschweig (Germany)
University of Copenhagen (Denmark)
University of Bern (Switzerland)
Argonne National Laboratory (ANL), Argonne, IL (United States)
Technical University of Denmark, Lyngby (Denmark)

Iridium nanoparticles are important catalysts for several chemical and energy conversion reactions. Studies of iridium nanoparticles have also been a key for the development of kinetic models of nanomaterial formation. However, compared to other metals such as gold or platinum, knowledge on the nature of prenucleation species and structural insights into the resultant nanoparticles are missing, especially for nanoparticles obtained from Ir$$_x$$Cl$$_y$$ precursors investigated here. We use in situ X-ray total scattering (TS) experiments with pair distribution function (PDF) analysis to study a simple, surfactant-free synthesis of colloidal iridium nanoparticles. The reaction is performed in methanol at 50 °C with only a base and an iridium salt as precursor. From different precursor salts–IrCl₃, IrCl₄, H₂IrCl₆, or Na₂IrCl₆–colloidal nanoparticles as small as Ir_~55 are obtained as the final product. The nanoparticles do not show the bulk iridium face-centered cubic ($fcc$) structure but show decahedral and icosahedral structures. The formation route is highly dependent on the precursor salt used. Using IrCl₃ or IrCl₄, metallic iridium nanoparticles form rapidly from Ir$$_x$$Cl$$_y$$$$^{n–}$$ complexes, whereas using H₂IrCl₆ or Na₂IrCl₆, the iridium nanoparticle formation follows a sudden growth after an induction period and the brief appearance of a crystalline phase. With H₂IrCl₆, the formation of different Ir$$_n$$ ($$n$$ = 55, 55, 85, and 116) nanoparticles depends on the nature of the cation in the base (LiOH, NaOH, KOH, or CsOH, respectively) and larger particles are obtained with larger cations. As the particles grow, the nanoparticle structure changes from partly icosahedral to decahedral. In conclusion, the results show that the synthesis of iridium nanoparticles from Ir$$_x$$Cl$$_y$$ is a valuable iridium nanoparticle model system, which can provide new compositional and structural insights into iridium nanoparticle formation and growth.

View Accepted Manuscript (DOE)

Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 2000031

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 3 Vol. 145; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Facile Synthesis of Ligand-Free Iridium Nanoparticles and Their In Vitro Biocompatibility Brown, Anna; Winter, Hayden; Goforth, Andrea figshare https://doi.org/10.6084/m9.figshare.c.4165493.v1	collection	January 2018

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