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Unravelling the synthesis mechanism of colloidal InP nanocrystals

Kim De Nolf UGent, Mickaël Tessier UGent, Dorian Dupont UGent, Jonathan De Roo UGent, Davy Sinnaeve UGent, Pieter Surmont UGent, José Martins UGent and Zeger Hens UGent (2015) Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts.
abstract
Colloidal semiconductor nanocrystals or quantum dots (QDs) are a class of materials that offer various promising applications in fields related to light emission and absorption. Most studied nanocrystals active at visible wavelengths involve cadmium chalcogenide based materials. However, cadmium is a toxic heavy metal that is restricted in several countries. Consequently, to make the use of QDs feasible, interest is shifting from the well-characterized Cd chalcogenide QDs to Cd-free alternatives such as CuInS2 or InP. Here especially InP QDs combine emission characteristics that come close to CdSe QDs with a reduced toxicity. Recently a synthesis protocol based on indium halide and tris(diethylamino)phosphine precusors in oleylamine as a solvent was introduced that will allow for an economic, up-scaled production of InP quantum dots (QDs).1 The reaction attains a close to full yield conversion − with respect to the indium precursor − and size tuning at full chemical yield is possible by changing the nature of the indium halide salt. Here, we unravel the mechanism by which the In and P react to form InP in this new synthesis by using high resolution NMR spectroscopy. First, 31P NMR measurements reveal how the diethylamino groups of the tris(diethylamino)phosphine precursor are exchanged for oleylamino groups. Additionally, a phosphorous containing reaction byproduct is detected in the NMR spectra, whose formation matches the InP formation rate. By means of 31P diffusion ordered spectroscopy (31P DOSY) and mass spectroscopy measurements, this byproduct is identified. Subsequently the synthesis mechanism was resolved: 3 aminophosphines out of 4 act as reducing agent for the remaining aminophosphine to yield one InP unit. This acquired knowledge allows for future research to focus on finding an alternative reducing agent to make the synthesis more efficient in terms of precursor use.
Please use this url to cite or link to this publication:
author
organization
year
type
conference (meetingAbstract)
publication status
published
subject
in
Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts
conference name
14th Young Belgian Magnetic Resonance Scientist (YBMRS) symposium
conference location
Blankenberge, Belgium
conference start
2015-11-30
conference end
2015-12-01
language
English
UGent publication?
yes
classification
C3
id
7072172
handle
http://hdl.handle.net/1854/LU-7072172
date created
2016-02-04 12:54:13
date last changed
2017-06-20 11:20:12
@inproceedings{7072172,
  abstract     = {Colloidal semiconductor nanocrystals or quantum dots (QDs) are a class of materials that offer various promising applications in fields related to light emission and absorption. Most studied nanocrystals active at visible wavelengths involve cadmium chalcogenide based materials. However, cadmium is a toxic heavy metal that is restricted in several countries. Consequently, to make the use of QDs feasible, interest is shifting from the well-characterized Cd chalcogenide QDs to Cd-free alternatives such as CuInS2 or InP. Here especially InP QDs combine emission characteristics that come close to CdSe QDs with a reduced toxicity. 
Recently a synthesis protocol based on indium halide and tris(diethylamino)phosphine precusors in oleylamine as a solvent was introduced that will allow for an economic, up-scaled production of InP quantum dots (QDs).1 The reaction attains a close to full yield conversion \ensuremath{-} with respect to the indium precursor \ensuremath{-} and size tuning at full chemical yield is possible by changing the nature of the indium halide salt. 
Here, we unravel the mechanism by which the In and P react to form InP in this new synthesis by using high resolution NMR spectroscopy. First, 31P NMR measurements reveal how the diethylamino groups of the tris(diethylamino)phosphine precursor are exchanged for oleylamino groups. Additionally, a phosphorous containing reaction byproduct is detected in the NMR spectra, whose formation matches the InP formation rate. By means of 31P diffusion ordered spectroscopy (31P DOSY) and mass spectroscopy measurements, this byproduct is identified. Subsequently the synthesis mechanism was resolved: 3 aminophosphines out of 4 act as reducing agent for the remaining aminophosphine to yield one InP unit. This acquired knowledge allows for future research to focus on finding an alternative reducing agent to make the synthesis more efficient in terms of precursor use.},
  author       = {De Nolf, Kim and Tessier, Micka{\"e}l and Dupont, Dorian and De Roo, Jonathan and Sinnaeve, Davy and Surmont, Pieter and Martins, Jos{\'e} and Hens, Zeger},
  booktitle    = {Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts},
  language     = {eng},
  location     = {Blankenberge, Belgium},
  title        = {Unravelling the synthesis mechanism of colloidal InP nanocrystals},
  year         = {2015},
}

Chicago
De Nolf, Kim, Mickaël Tessier, Dorian Dupont, Jonathan De Roo, Davy Sinnaeve, Pieter Surmont, José Martins, and Zeger Hens. 2015. “Unravelling the Synthesis Mechanism of Colloidal InP Nanocrystals.” In Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts.
APA
De Nolf, K., Tessier, M., Dupont, D., De Roo, J., Sinnaeve, D., Surmont, P., Martins, J., et al. (2015). Unravelling the synthesis mechanism of colloidal InP nanocrystals. Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts. Presented at the 14th Young Belgian Magnetic Resonance Scientist (YBMRS) symposium.
Vancouver
1.
De Nolf K, Tessier M, Dupont D, De Roo J, Sinnaeve D, Surmont P, et al. Unravelling the synthesis mechanism of colloidal InP nanocrystals. Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts. 2015.
MLA
De Nolf, Kim, Mickaël Tessier, Dorian Dupont, et al. “Unravelling the Synthesis Mechanism of Colloidal InP Nanocrystals.” Young Belgian Magnetic Resonance Scientist, 14th Symposium, Abstracts. 2015. Print.