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Insights into Nucleation and Growth of Colloidal Quaternary Nanocrystals by Multimodal X-ray Analysis

Just, Justus LU ; Coughlan, Claudia ; Singh, Shalini ; Ren, Huan ; Müller, Oliver ; Becker, Pascal ; Unold, Thomas and Ryan, Kevin M. (2021) In ACS Nano 15(4). p.6439-6447
Abstract

Copper chalcogenide nanocrystals find applications in photovoltaic inks, bio labels, and thermoelectric materials. We reveal insights in the nucleation and growth during synthesis of anisotropic Cu2ZnSnS4 nanocrystals by simultaneously performing in situ X-ray absorption spectroscopy (XAS) and small-angle X-ray scattering (SAXS). Real-time XAFS reveals that upon thiol injection into the reaction flask, a key copper thiolate intermediate species is formed within fractions of seconds, which decomposes further within a narrow temperature and time window to form copper sulfide nanocrystals. These nanocrystals convert into Cu2ZnSnS4 nanorods by sequentially incorporating Sn and Zn. Real-time SAXS and ex situ TEM of aliquots corroborate these... (More)

Copper chalcogenide nanocrystals find applications in photovoltaic inks, bio labels, and thermoelectric materials. We reveal insights in the nucleation and growth during synthesis of anisotropic Cu2ZnSnS4 nanocrystals by simultaneously performing in situ X-ray absorption spectroscopy (XAS) and small-angle X-ray scattering (SAXS). Real-time XAFS reveals that upon thiol injection into the reaction flask, a key copper thiolate intermediate species is formed within fractions of seconds, which decomposes further within a narrow temperature and time window to form copper sulfide nanocrystals. These nanocrystals convert into Cu2ZnSnS4 nanorods by sequentially incorporating Sn and Zn. Real-time SAXS and ex situ TEM of aliquots corroborate these findings. Our work demonstrates how combined in situ X-ray absorption and small-angle X-ray scattering enables the understanding of mechanistic pathways in colloidal nanocrystal formation.

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author
; ; ; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
colloidal nanocrystals, CZTS, in situ EXAFS/XANES/SAXS, nucleation and growth, quick-EXAFS, wurtzite
in
ACS Nano
volume
15
issue
4
pages
6439 - 6447
publisher
The American Chemical Society (ACS)
external identifiers
  • pmid:33770436
  • scopus:85104961968
ISSN
1936-0851
DOI
10.1021/acsnano.0c08617
language
English
LU publication?
yes
id
1d2c0528-2ada-48a8-aac2-4eed3eb3e3c8
date added to LUP
2021-05-10 15:20:37
date last changed
2024-06-29 12:05:19
@article{1d2c0528-2ada-48a8-aac2-4eed3eb3e3c8,
  abstract     = {{<p>Copper chalcogenide nanocrystals find applications in photovoltaic inks, bio labels, and thermoelectric materials. We reveal insights in the nucleation and growth during synthesis of anisotropic Cu2ZnSnS4 nanocrystals by simultaneously performing in situ X-ray absorption spectroscopy (XAS) and small-angle X-ray scattering (SAXS). Real-time XAFS reveals that upon thiol injection into the reaction flask, a key copper thiolate intermediate species is formed within fractions of seconds, which decomposes further within a narrow temperature and time window to form copper sulfide nanocrystals. These nanocrystals convert into Cu2ZnSnS4 nanorods by sequentially incorporating Sn and Zn. Real-time SAXS and ex situ TEM of aliquots corroborate these findings. Our work demonstrates how combined in situ X-ray absorption and small-angle X-ray scattering enables the understanding of mechanistic pathways in colloidal nanocrystal formation. </p>}},
  author       = {{Just, Justus and Coughlan, Claudia and Singh, Shalini and Ren, Huan and Müller, Oliver and Becker, Pascal and Unold, Thomas and Ryan, Kevin M.}},
  issn         = {{1936-0851}},
  keywords     = {{colloidal nanocrystals; CZTS; in situ EXAFS/XANES/SAXS; nucleation and growth; quick-EXAFS; wurtzite}},
  language     = {{eng}},
  number       = {{4}},
  pages        = {{6439--6447}},
  publisher    = {{The American Chemical Society (ACS)}},
  series       = {{ACS Nano}},
  title        = {{Insights into Nucleation and Growth of Colloidal Quaternary Nanocrystals by Multimodal X-ray Analysis}},
  url          = {{http://dx.doi.org/10.1021/acsnano.0c08617}},
  doi          = {{10.1021/acsnano.0c08617}},
  volume       = {{15}},
  year         = {{2021}},
}