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A High Yield Synthesis of Ligand-Free Iridium Oxide Nanoparticles with High Electrocatalytic Activity

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Department of Chemistry, The Pennsylvania State University, University Park, Pennsylvania, 16802, United States
Cite this: J. Phys. Chem. Lett. 2011, 2, 5, 402–406
Publication Date (Web):February 7, 2011
Copyright © 2011 American Chemical Society

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    Stable blue suspensions of 2 nm diameter iridium oxide (IrOx·nH2O) nanoparticles were obtained by hydrolyzing IrCl62− in base at 90 °C to produce [Ir(OH)6]2− and then treating with HNO3 at 0 °C. UV−visible spectra show that acid condensation of [Ir(OH)6]2− results in quantitative conversion to stable, ligand-free IrOx·nH2O nanoparticles, which have an extinction coefficient of 630 ± 50 M−1cm−1 at 580 nm. In contrast, alkaline hydrolysis alone converts only 30% of the sample to IrOx·nH2O at 2 mM concentration. The acidified nanoparticles are stable for at least one month at 2 °C and can be used to make colloidal solutions between pH 1 and 13. At pH 7 and above, some hydrolysis to form [Ir(OH)6]2− occurs. Uniform IrOx·nH2O electrode films were grown anodically from pH 1 solutions, and were found to be highly active for water oxidation between pH 1 and 13.

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    UV−visible spectra of acidic IrOx·nH2O colloids prepared using HBF4 and HCl in place of HNO3, TEM images of IrOx·nH2O nanoparticles, photographs of FTO electrodes with colloidal IrOx·nH2O films, and electrochemical data from RDE experiments (5 pp). This material is available free of charge via the Internet at

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