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
Abstract
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.
- Authors:
-
[2];
[3];
[3];
[4];
[5];
[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)
- Publication Date:
- Research Org.:
- Argonne National Laboratory (ANL), Argonne, IL (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)
- OSTI Identifier:
- 2000031
- Grant/Contract Number:
- AC02-06CH11357
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of the American Chemical Society
- Additional Journal Information:
- Journal Volume: 145; Journal Issue: 3; Journal ID: ISSN 0002-7863
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; chemical structure; crystal structure; metals; precursors; transition metals
Citation Formats
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, and Jensen, Kirsten M. Ø. 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. United States: N. p., 2023.
Web. doi:10.1021/jacs.2c10814.
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. 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. United States. https://doi.org/10.1021/jacs.2c10814
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, and Jensen, Kirsten M. Ø. Wed .
"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". United States. https://doi.org/10.1021/jacs.2c10814. https://www.osti.gov/servlets/purl/2000031.
@article{osti_2000031,
title = {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},
author = {Mathiesen, Jette K. and Quinson, Jonathan and Blaseio, Sonja and Kjær, Emil T. S. and Dworzak, Alexandra and Cooper, Susan R. and Pedersen, Jack K. and Wang, Baiyu and Bizzotto, Francesco and Schröder, Johanna and Kinnibrugh, Tiffany L. and Simonsen, Søren B. and Theil Kuhn, Luise and Kirkensgaard, Jacob J. K. and Rossmeisl, Jan and Oezaslan, Mehtap and Arenz, Matthias and Jensen, Kirsten M. Ø.},
abstractNote = {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.},
doi = {10.1021/jacs.2c10814},
journal = {Journal of the American Chemical Society},
number = 3,
volume = 145,
place = {United States},
year = {Wed Jan 11 00:00:00 EST 2023},
month = {Wed Jan 11 00:00:00 EST 2023}
}
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- Hammersley, A. P.; Svensson, S. O.; Hanfland, M.
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FIT2D : a multi-purpose data reduction, analysis and visualization program
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A Critical Size for Emergence of Nonbulk Electronic and Geometric Structures in Dodecanethiolate-Protected Au Clusters
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