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Elucidating the Location of Cd2+ in Post-synthetically Treated InP Quantum Dots Using Dynamic Nuclear Polarization 31P and 113Cd Solid-State NMR Spectroscopy

Journal Article · · Journal of Physical Chemistry. C

Indium phosphide quantum dots (InP QD) are a promising alternative to traditional QD materials that contain toxic heavy elements such as lead and cadmium. However, InP QD obtained from colloidal synthesis are often plagued by poor photoluminescence quantum yields (PL-QYs). In order to improve the PL-QY of InP QD, a number of post-synthetic treatments have been devised. Recently, it has been shown that InP post-synthetically treated with Lewis acid metal divalent cations (M-InP) exhibit enhanced PL-QY; however, the molecular structure and mechanism behind the improved PL-QY are not fully understood. Here, to determine the surface structure of M-InP QD, dynamic nuclear polarization surface-enhanced nuclear magnetic resonance spectroscopy (DNP SENS) experiments were employed on a series of InP magic size clusters treated with Cd ions, InP QD, cadmium phosphide (Cd3P2) QD, and Cd-treated InP QD (Cd–InP QD). With the use of DNP SENS, we were able to obtain the 1D 31P and 113Cd NMR spectra, 113Cd{31P} rotational-echo double-resonance (REDOR) NMR spectra, and 31P{113Cd} dipolar heteronuclear multiple quantum correlation (D-HMQC) sequence. Changes in the phosphide 31P chemical shifts after Cd treatment provide indirect evidence that some Cd alloys into the sub-surface regions of the particle. DNP-enhanced 113Cd solid-state NMR spectra suggest that most Cd ions are coordinated by oxygen atoms from either carboxylate ligands or surface phosphate groups. 113Cd{31P} REDOR and 31P{113Cd} D-HMQC experiments confirm that a subset of Cd ions are located on the surface of Cd–InP QD and coordinated with phosphate groups.

Research Organization:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division; Alfred P. Sloan Foundation; National Science Foundation (NSF)
Grant/Contract Number:
AC02-07CH11358
OSTI ID:
1764374
Report Number(s):
IS--J-10,405
Journal Information:
Journal of Physical Chemistry. C, Journal Name: Journal of Physical Chemistry. C Journal Issue: 5 Vol. 125; ISSN 1932-7447
Publisher:
American Chemical SocietyCopyright Statement
Country of Publication:
United States
Language:
English

References (66)

Beyond the Silica Surface by Direct Silicon-29 Dynamic Nuclear Polarization journal July 2011
Frozen Acrylamide Gels as Dynamic Nuclear Polarization Matrices journal June 2017
Analytic Solutions for the Time Evolution of Dipolar-Dephasing NMR Signals journal March 1995
An Improved Broadband Decoupling Sequence for Liquid Crystals and Solids journal January 2000
The structure of the compound Cd3P2 journal January 2006
Total suppression of sidebands in CPMAS C-13 NMR journal September 1982
Rotational-echo double-resonance NMR journal January 1989
13C/14N heteronuclear multiple-quantum correlation with rotary resonance and REDOR dipolar recoupling journal January 2007
Reactions of Cd(OAc)2·2H2O with variously substituted pyridines. Efforts to unravel the factors that determine structure/nuclearity of the products journal September 2015
Endogenous dynamic nuclear polarization NMR of hydride-terminated silicon nanoparticles journal August 2019
Identifying the Molecular Edge Termination of Exfoliated Hexagonal Boron Nitride Nanosheets with Solid-State NMR Spectroscopy and Plane-Wave DFT Calculations journal February 2020
Two-Step Nucleation and Growth of InP Quantum Dots via Magic-Sized Cluster Intermediates journal February 2015
Chemistry of InP Nanocrystal Syntheses journal April 2016
Cation Exchange Induced Transformation of InP Magic-Sized Clusters journal September 2017
Probing Surface Defects of InP Quantum Dots Using Phosphorus Kα and Kβ X-ray Emission Spectroscopy journal August 2018
Interfacial Oxidation and Photoluminescence of InP-Based Core/Shell Quantum Dots journal September 2018
Formation of Size-Tunable and Nearly Monodisperse InP Nanocrystals: Chemical Reactions and Controlled Synthesis journal June 2019
Synthesis of Semiconductor Nanocrystals, Focusing on Nontoxic and Earth-Abundant Materials journal July 2016
Elucidating the Location of Cd 2+ in Post-synthetically Treated InP Quantum Dots Using Dynamic Nuclear Polarization 31 P and 113 Cd Solid-State NMR Spectroscopy journal January 2021
NMR and EPR Characterization of Functionalized Nanodiamonds journal May 2015
Luminescent InP Quantum Dots with Tunable Emission by Post-Synthetic Modification with Lewis Acids journal March 2016
Purification and In Situ Ligand Exchange of Metal-Carboxylate-Treated Fluorescent InP Quantum Dots via Gel Permeation Chromatography journal August 2017
Synthesis and Degradation of Cadmium-Free InP and InPZn/ZnS Quantum Dots in Solution journal October 2018
Colloidal-ALD-Grown Core/Shell CdSe/CdS Nanoplatelets as Seen by DNP Enhanced PASS–PIETA NMR Spectroscopy journal February 2020
Mesoporous Silica-Supported Amidozirconium-Catalyzed Carbonyl Hydroboration journal November 2015
Dynamic Nuclear Polarization Solid-State NMR in Heterogeneous Catalysis Research journal October 2015
Resolving the Core and the Surface of CdSe Quantum Dots and Nanoplatelets Using Dynamic Nuclear Polarization Enhanced PASS–PIETA NMR Spectroscopy journal June 2018
High Frequency Dynamic Nuclear Polarization journal April 2013
Role of Acid in Precursor Conversion During InP Quantum Dot Synthesis journal June 2013
Studies of Organically Functionalized Mesoporous Silicas Using Heteronuclear Solid-State Correlation NMR Spectroscopy under Fast Magic Angle Spinning journal May 2005
Colloidal InP Nanocrystals as Efficient Emitters Covering Blue to Near-Infrared journal December 2007
Surface Chemistry of InP Quantum Dots: A Comprehensive Study journal December 2010
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization journal November 2010
Surface-Amplified Ligand Disorder in CdSe Quantum Dots Determined by Electron and Coherent Vibrational Spectroscopies journal May 2011
InP/ZnS Nanocrystals: Coupling NMR and XPS for Fine Surface and Interface Description journal November 2012
Improved Precursor Chemistry for the Synthesis of III–V Quantum Dots journal December 2012
Large Molecular Weight Nitroxide Biradicals Providing Efficient Dynamic Nuclear Polarization at Temperatures up to 200 K journal August 2013
Ligand Exchange and the Stoichiometry of Metal Chalcogenide Nanocrystals: Spectroscopic Observation of Facile Metal-Carboxylate Displacement and Binding
  • Anderson, Nicholas C.; Hendricks, Mark P.; Choi, Joshua J.
  • Journal of the American Chemical Society, Vol. 135, Issue 49, p. 18536-18548 https://doi.org/10.1021/ja4086758
journal November 2013
Size- and Site-Dependent Reconstruction in CdSe QDs Evidenced by 77 Se{ 1 H} CP-MAS NMR Spectroscopy journal March 2010
Synthesis and Characterization of Cadmium Phosphide Quantum Dots Emitting in the Visible Red to Near-Infrared journal April 2010
Structure of Colloidal Quantum Dots from Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy journal October 2015
Bulk Nuclear Hyperpolarization of Inorganic Solids by Relay from the Surface journal May 2018
Probing the Surface Structure of Semiconductor Nanoparticles by DNP SENS with Dielectric Support Materials journal August 2019
Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13 C and 29 Si NMR Enhanced by Dynamic Nuclear Polarization journal January 2013
Primostrato Solid-State NMR Enhanced by Dynamic Nuclear Polarization: Pentacoordinated Al 3+ Ions Are Only Located at the Surface of Hydrated γ-Alumina journal October 2014
A 31 P Spin Diffusion and 31 P− 113 Cd CP/MAS NMR Study of Polycrystalline Cd 3 (PO 4 ) 2 journal August 1997
Unraveling the Core–Shell Structure of Ligand-Capped Sn/SnO x Nanoparticles by Surface-Enhanced Nuclear Magnetic Resonance, Mössbauer, and X-ray Absorption Spectroscopies journal February 2014
Prospects of Nanoscience with Nanocrystals journal January 2015
Direct probe of spectral inhomogeneity reveals synthetic tunability of single-nanocrystal spectral linewidths journal June 2013
Rapid synthesis of highly luminescent InP and InP/ZnS nanocrystals journal January 2008
Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results journal January 2010
Non-aqueous solvents for DNP surface enhanced NMR spectroscopy journal January 2012
Indirect and direct 29 Si dynamic nuclear polarization of dispersed nanoparticles journal January 2013
Dynamic nuclear polarization of spherical nanoparticles journal January 2013
From discrete molecule, to polymer, to MOF: mapping the coordination chemistry of Cd II using 113 Cd solid-state NMR journal January 2016
Surface-selective direct 17 O DNP NMR of CeO 2 nanoparticles journal January 2017
Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences journal January 2016
Gel permeation chromatography as a multifunctional processor for nanocrystal purification and on-column ligand exchange chemistry journal January 2016
Broadband dipolar recoupling in the nuclear magnetic resonance of rotating solids: A compensated C7 pulse sequence journal February 1998
NMR study of InP quantum dots: Surface structure and size effects journal May 1999
Scalar and anisotropic J interactions in undoped InP: A triple-resonance NMR study journal October 1998
Atomic Positional Versus Electronic Order in Semiconducting ZnSe Nanoparticles journal September 2009
NMR Study of Semiconductor Molecular Clusters journal June 1988
The coordination chemistry of nanocrystal surfaces journal February 2015
NMR nomenclature. Nuclear spin properties and conventions for chemical shifts(IUPAC Recommendations 2001) journal January 2001
Synthesis of In37P20(O2CR)51 Clusters and Their Conversion to InP Quantum Dots journal January 2019

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