Issue 23, 2024

Troubleshooting the influence of trace chemical impurities on nanoparticle growth kinetics via electrochemical measurements

Abstract

Reproducibility issues resulting from particle growth solutions made with cetyltrimethylammonium bromide (CTAB) surfactant from different lots and product lines in a newly developed synthesis of monometallic palladium (Pd) tetrahexahedra (THH) nanoparticles are investigated via a multi-pronged approach. Time-resolved electrochemical measurements of solution potential, variation of chemical parameters in colloidal synthesis, and correlation to electrodeposition syntheses are used together to uncover the effects of the unknown contaminants on the chemical reducing environment during nanoparticle growth. Iodide—a known impurity in commercial CTAB—is identified as one of the required components for equalizing the reducing environment across multiple CTAB sources. However, an additional component—acetone—is critical to establishing the growth kinetics necessary to enable the reproducible synthesis of THH in each of the CTAB formulations. In one CTAB variety, the powdered surfactant contains too much acetone, and drying of the as-received surfactant and re-addition of solvent is necessary for successful Pd THH synthesis. The relevance of solvent impurities to the reducing environment in aqueous nanoparticle synthesis is confirmed via electrochemical measurement approaches and solvent addition experiments. This work highlights the utility of real-time electrochemical potential measurements as a tool for benchmarking of nanoparticle syntheses and troubleshooting of reproducibility issues. The results additionally emphasize the importance of considering organic solvent impurities in powdered commercial reagents as a possible shape-determining factor during shaped nanomaterials synthesis.

Graphical abstract: Troubleshooting the influence of trace chemical impurities on nanoparticle growth kinetics via electrochemical measurements

Supplementary files

Article information

Article type
Paper
Submitted
05 jan 2024
Accepted
24 apr 2024
First published
25 apr 2024
This article is Open Access
Creative Commons BY-NC license

Nanoscale, 2024,16, 11038-11051

Troubleshooting the influence of trace chemical impurities on nanoparticle growth kinetics via electrochemical measurements

G. C. Halford, S. P. McDarby, S. Hertle, A. F. Kiely, J. T. Luu, C. J. Wang and M. L. Personick, Nanoscale, 2024, 16, 11038 DOI: 10.1039/D4NR00070F

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