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Protesescu L, Rossini AJ, Kriegner D, et al. Unraveling the core-shell structure of ligand-capped Sn/SnOx nanoparticles by surface-enhanced nuclear magnetic resonance, Mössbauer, and X-ray absorption spectroscopies. ACS Nano. 2014;8(3):2639-48doi: 10.1021/nn406344n.
Protesescu, L., Rossini, A. J., Kriegner, D., Valla, M., de Kergommeaux, A., Walter, M., Kravchyk, K. V., Nachtegaal, M., Stangl, J., Malaman, B., Reiss, P., Lesage, A., Emsley, L., Copéret, C., & Kovalenko, M. V. (2014). Unraveling the core-shell structure of ligand-capped Sn/SnOx nanoparticles by surface-enhanced nuclear magnetic resonance, Mössbauer, and X-ray absorption spectroscopies. ACS nano, 8(3), 2639-48. https://doi.org/10.1021/nn406344n
Protesescu, Loredana, et al. "Unraveling the core-shell structure of ligand-capped Sn/SnOx nanoparticles by surface-enhanced nuclear magnetic resonance, Mössbauer, and X-ray absorption spectroscopies." ACS nano vol. 8,3 (2014): 2639-48. doi: https://doi.org/10.1021/nn406344n
Protesescu L, Rossini AJ, Kriegner D, Valla M, de Kergommeaux A, Walter M, Kravchyk KV, Nachtegaal M, Stangl J, Malaman B, Reiss P, Lesage A, Emsley L, Copéret C, Kovalenko MV. Unraveling the core-shell structure of ligand-capped Sn/SnOx nanoparticles by surface-enhanced nuclear magnetic resonance, Mössbauer, and X-ray absorption spectroscopies. ACS Nano. 2014 Mar 25;8(3):2639-48. doi: 10.1021/nn406344n. Epub 2014 Feb 04. PMID: 24494636.
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ACS Nano. 2014 Mar 25;8(3):2639-48. doi: 10.1021/nn406344n. Epub 2014 Feb 04.

Unraveling the core-shell structure of ligand-capped Sn/SnOx nanoparticles by surface-enhanced nuclear magnetic resonance, Mössbauer, and X-ray absorption spectroscopies.

ACS nano

Loredana Protesescu, Aaron J Rossini, Dominik Kriegner, Maxence Valla, Antoine de Kergommeaux, Marc Walter, Kostiantyn V Kravchyk, Maarten Nachtegaal, Julian Stangl, Bernard Malaman, Peter Reiss, Anne Lesage, Lyndon Emsley, Christophe Copéret, Maksym V Kovalenko

Affiliations

  1. Institute of Inorganic Chemistry, Department of Chemistry and Applied Biosciences, ETH Zürich CH-8093, Switzerland.

PMID: 24494636 DOI: 10.1021/nn406344n

Abstract

A particularly difficult challenge in the chemistry of nanomaterials is the detailed structural and chemical analysis of multicomponent nano-objects. This is especially true for the determination of spatially resolved information. In this study, we demonstrate that dynamic nuclear polarization surface-enhanced solid-state NMR spectroscopy (DNP-SENS), which provides selective and enhanced NMR signal collection from the (near) surface regions of a sample, can be used to resolve the core-shell structure of a nanoparticle. Li-ion anode materials, monodisperse 10-20 nm large tin nanoparticles covered with a ∼3 nm thick layer of native oxides, were used in this case study. DNP-SENS selectively enhanced the weak 119Sn NMR signal of the amorphous surface SnO2 layer. Mössbauer and X-ray absorption spectroscopies identified a subsurface SnO phase and quantified the atomic fractions of both oxides. Finally, temperature-dependent X-ray diffraction measurements were used to probe the metallic β-Sn core and indicated that even after 8 months of storage at 255 K there are no signs of conversion of the metallic β-Sn core into a brittle semiconducting α-phase, a phase transition which normally occurs in bulk tin at 286 K (13 °C). Taken together, these results indicate that Sn/SnOx nanoparticles have core/shell1/shell2 structure of Sn/SnO/SnO2 phases. The study suggests that DNP-SENS experiments can be carried on many types of uniform colloidal nanomaterials containing NMR-active nuclei, in the presence of either hydrophilic (ion-capped surfaces) or hydrophobic (capping ligands with long hydrocarbon chains) surface functionalities.

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