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De Roo J, Coucke S, Rijckaert H, et al. Amino Acid-Based Stabilization of Oxide Nanocrystals in Polar Media: From Insight in Ligand Exchange to Solution ¹H NMR Probing of Short-Chained Adsorbates. Langmuir. 2016;32(8):1962-70doi: 10.1021/acs.langmuir.5b04611.
De Roo, J., Coucke, S., Rijckaert, H., De Keukeleere, K., Sinnaeve, D., Hens, Z., Martins, J. C., & Van Driessche, I. (2016). Amino Acid-Based Stabilization of Oxide Nanocrystals in Polar Media: From Insight in Ligand Exchange to Solution ¹H NMR Probing of Short-Chained Adsorbates. Langmuir : the ACS journal of surfaces and colloids, 32(8), 1962-70. https://doi.org/10.1021/acs.langmuir.5b04611
De Roo, Jonathan, et al. "Amino Acid-Based Stabilization of Oxide Nanocrystals in Polar Media: From Insight in Ligand Exchange to Solution ¹H NMR Probing of Short-Chained Adsorbates." Langmuir : the ACS journal of surfaces and colloids vol. 32,8 (2016): 1962-70. doi: https://doi.org/10.1021/acs.langmuir.5b04611
De Roo J, Coucke S, Rijckaert H, De Keukeleere K, Sinnaeve D, Hens Z, Martins JC, Van Driessche I. Amino Acid-Based Stabilization of Oxide Nanocrystals in Polar Media: From Insight in Ligand Exchange to Solution ¹H NMR Probing of Short-Chained Adsorbates. Langmuir. 2016 Mar 01;32(8):1962-70. doi: 10.1021/acs.langmuir.5b04611. Epub 2016 Feb 17. PMID: 26854070.
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Langmuir. 2016 Mar 01;32(8):1962-70. doi: 10.1021/acs.langmuir.5b04611. Epub 2016 Feb 17.

Amino Acid-Based Stabilization of Oxide Nanocrystals in Polar Media: From Insight in Ligand Exchange to Solution ¹H NMR Probing of Short-Chained Adsorbates.

Langmuir : the ACS journal of surfaces and colloids

Jonathan De Roo, Sofie Coucke, Hannes Rijckaert, Katrien De Keukeleere, Davy Sinnaeve, Zeger Hens, José C Martins, Isabel Van Driessche

Affiliations

  1. Sol-Gel Center for Research on Inorganic Powders and Thin films Synthesis (SCRiPTS), ‡Physics and Chemistry of Nanostructures group (PCN), §NMR and Structure Analysis Unit (NMRSTR), ?Center for Nano and Biophotonics, Ghent University , 9000 Ghent, Belgium.

PMID: 26854070 DOI: 10.1021/acs.langmuir.5b04611

Abstract

Ligand exchange is a crucial step between nanocrystal synthesis and nanocrystal application. Although colloidal stability and ligand exchange in nonpolar media are readily established, the exchange of native, hydrophobic ligands with polar ligands is less systematic. In this paper, we present a versatile ligand exchange strategy for the phase transfer of carboxylic acid capped HfO2 and ZrO2 nanocrystals to various polar solvents, based on small amino acids as the incoming ligand. To gain insight in the fundamental mechanism of the exchange, we study this system with a combination of FTIR, zeta potential measurements, and solution (1)H NMR techniques. The detection of surface-associated, small ligands with solution NMR proves challenging in this respect. Tightly bound amino acids are undetectable, but their existence can be proven through displacement with other ligands in titration experiments. Alternatively, we find that methyl moieties belonging to bound species can circumvent these limitations because of their more favorable relaxation properties as a result of internal mobility. As such, our results are not limited to amino acids but to any short-chained ligand and will therefore facilitate the rigorous investigation and understanding of various ligand exchange processes.

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