Revealing the Surface Structure of CdSe Nanocrystals by Dynamic Nuclear Polarization-Enhanced 77Se and 113Cd Solid-State NMR Spectroscopy

Chen, Yunhua; Dorn, Rick W.; Hanrahan, Michael P.; Wei, Lin; Blome-Fernández, Rafael; Medina-Gonzalez, Alan M.; Adamson, Marquix S.; Flintgruber, Anne H.; Vela, Javier; Rossini, Aaron J.

doi:10.1021/jacs.1c03162

Revealing the Surface Structure of CdSe Nanocrystals by Dynamic Nuclear Polarization-Enhanced ⁷⁷Se and ¹¹³Cd Solid-State NMR Spectroscopy

Journal Article · Fri Jun 04 00:00:00 EDT 2021 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.1c03162· OSTI ID:1797579

Chen, Yunhua ^[1]; Dorn, Rick W. ^[1]; Hanrahan, Michael P. ^[1]; Wei, Lin ^[2]; Blome-Fernández, Rafael ^[2]; Medina-Gonzalez, Alan M. ^[2]; Adamson, Marquix S. ^[2]; Flintgruber, Anne H. ^[3]; ^[1]; ^[1]

Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States)
Iowa State Univ., Ames, IA (United States)
Ames Lab., Ames, IA (United States)

Dynamic nuclear polarization (DNP) solid-state NMR (SSNMR) spectroscopy was used to obtain detailed surface structures of zinc blende CdSe nanocrystals (NCs) with plate or spheroidal morphologies which are capped by carboxylic acid ligands. 1D ¹¹³Cd and ⁷⁷Se cross-polarization magic angle spinning (CPMAS) NMR spectra revealed distinct signals from Cd and Se atoms on the surface of the NCs, and those residing in bulk-like environments, below the surface. ¹¹³Cd cross-polarization magic-angle-turning (CP-MAT) experiments identified CdSe₃O, CdSe₂O₂, and CdSeO₃ Cd coordination environments on the surface of the NCs, where the oxygen atoms are presumably from coordinated carboxylate ligands. The sensitivity gain from DNP enabled natural isotopic abundance 2D homonuclear ¹¹³Cd–¹¹³Cd and ⁷⁷Se–⁷⁷Se and heteronuclear ¹¹³Cd–⁷⁷Se scalar correlation solid-state NMR experiments which revealed the connectivity of the Cd and Se atoms. Importantly, ⁷⁷Se{¹¹³Cd} scalar heteronuclear multiple quantum coherence (J-HMQC) experiments were used to selectively measure one-bond ⁷⁷Se–¹¹³Cd scalar coupling constants (¹J(⁷⁷Se, ¹¹³Cd)). With knowledge of ¹J(⁷⁷Se, ¹¹³Cd), heteronuclear ⁷⁷Se{¹¹³Cd} spin echo (J-resolved) NMR experiments were used to determine the number of Cd atoms bonded to Se atoms and vice versa. Furthermore, the J-resolved experiments directly confirmed that major Cd and Se surface species have CdSe₂O₂ and SeCd₄ stoichiometries, respectively. Considering the crystal structure of zinc blende CdSe and the similarity of the solid-state NMR data for the platelets and spheroids, we conclude that the surface of the spheroidal CdSe NCs is primarily composed of {100} facets. The methods outlined here will generally be applicable to obtain detailed surface structures of various main group semiconductor nanoparticles.

View Accepted Manuscript (DOE)

Research Organization:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1797579

Report Number(s):: is-j-10-506

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 23 Vol. 143; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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