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Aminophosphines : a double role in the synthesis of colloidal indium phosphide quantum dots

Mickaël Tessier (UGent) , Kim De Nolf (UGent) , Dorian Dupont (UGent) , Davy Sinnaeve (UGent) , Jonathan De Roo (UGent) and Zeger Hens (UGent)
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Abstract
Aminophosphines have recently emerged as economical, easy-to-implement precursors for making InP nanocrystals, which stand out as alternative Cd-free quantum dots for optoelectronic applications. Here, we present a complete investigation of the chemical reactions leading to InP formation starting from InCl3 and tris(dialkylamino)phosphines. Using nuclear magnetic resonance (NMR) spectroscopy and single crystal X-ray diffraction, we demonstrate that injection of the aminophosphine in the reaction mixture is followed by a transamination with oleylamine, the solvent of the reaction. In addition, mass spectrometry and NMR indicate that the formation of InP concurs with that of tetra(oleylamino)phosphonium chloride. The chemical yield of the InP formation agrees with this 4 P(+III) -> P(-III) + 3 P(+V) disproportionation reaction occurring, since full conversion of the In precursor was only attained for a 4:1 P/In ratio. Hence it underlines the double role, of the aminophosphine as both precursor and reducing agent. These new insights will guide further optimization of high quality InP quantum dots and might lead to the extension of synthetic protocols toward other pnictide nanocrystals.
Keywords
INP NANOCRYSTALS, LIGAND DISPLACEMENT, HOT INJECTION, SIZE, RECOMBINATION, MECHANISM, CATALYSIS, EMISSION, SOLUTE, ROUTE

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Citation

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Chicago
Tessier, Mickaël, Kim De Nolf, Dorian Dupont, Davy Sinnaeve, Jonathan De Roo, and Zeger Hens. 2016. “Aminophosphines : a Double Role in the Synthesis of Colloidal Indium Phosphide Quantum Dots.” Journal of the American Chemical Society 138 (18): 5923–5929.
APA
Tessier, M., De Nolf, K., Dupont, D., Sinnaeve, D., De Roo, J., & Hens, Z. (2016). Aminophosphines : a double role in the synthesis of colloidal indium phosphide quantum dots. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 138(18), 5923–5929.
Vancouver
1.
Tessier M, De Nolf K, Dupont D, Sinnaeve D, De Roo J, Hens Z. Aminophosphines : a double role in the synthesis of colloidal indium phosphide quantum dots. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY. 2016;138(18):5923–9.
MLA
Tessier, Mickaël, Kim De Nolf, Dorian Dupont, et al. “Aminophosphines : a Double Role in the Synthesis of Colloidal Indium Phosphide Quantum Dots.” JOURNAL OF THE AMERICAN CHEMICAL SOCIETY 138.18 (2016): 5923–5929. Print.
@article{8028704,
  abstract     = {Aminophosphines have recently emerged as economical, easy-to-implement precursors for making InP nanocrystals, which stand out as alternative Cd-free quantum dots for optoelectronic applications. Here, we present a complete investigation of the chemical reactions leading to InP formation starting from InCl3 and tris(dialkylamino)phosphines. Using nuclear magnetic resonance (NMR) spectroscopy and single crystal X-ray diffraction, we demonstrate that injection of the aminophosphine in the reaction mixture is followed by a transamination with oleylamine, the solvent of the reaction. In addition, mass spectrometry and NMR indicate that the formation of InP concurs with that of tetra(oleylamino)phosphonium chloride. The chemical yield of the InP formation agrees with this 4 P(+III) -{\textrangle} P(-III) + 3 P(+V) disproportionation reaction occurring, since full conversion of the In precursor was only attained for a 4:1 P/In ratio. Hence it underlines the double role, of the aminophosphine as both precursor and reducing agent. These new insights will guide further optimization of high quality InP quantum dots and might lead to the extension of synthetic protocols toward other pnictide nanocrystals.},
  author       = {Tessier, Micka{\"e}l and De Nolf, Kim and Dupont, Dorian and Sinnaeve, Davy and De Roo, Jonathan and Hens, Zeger},
  issn         = {0002-7863},
  journal      = {JOURNAL OF THE AMERICAN CHEMICAL SOCIETY},
  keyword      = {INP NANOCRYSTALS,LIGAND DISPLACEMENT,HOT INJECTION,SIZE,RECOMBINATION,MECHANISM,CATALYSIS,EMISSION,SOLUTE,ROUTE},
  language     = {eng},
  number       = {18},
  pages        = {5923--5929},
  title        = {Aminophosphines : a double role in the synthesis of colloidal indium phosphide quantum dots},
  url          = {http://dx.doi.org/10.1021/jacs.6b01254},
  volume       = {138},
  year         = {2016},
}

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