Paper
Dalton Transactions
between the nitrogen atom of TOA and the NCs are clearly
evident in the NMR spectra of the InSb NCs coated with TOA
(Fig. 3b). Not only are the proton signals broad but also they
are chemically shifted downfield. For example, a chemical
shift of about 0.6 ppm was observed for protons on the
carbon-1 atom. Progressively smaller chemical shifts for
higher protons (carbon-2, -3, -4 etc.) were observed indicative
of the inductive effect. The presence of surface oxides was also
evident in Sb 3d core level spectra. Besides InSb (Sb 3d5/2
527.8 eV), the signals from Sb-oxide (Sb 3d5/2 530 eV) are
clearly visible. The O 1s signal overlaps with Sb 3d and is
assigned at 531.5 eV. The presence of oxides of both In and Sb
in the InSb sample is consistent with the literature reports.27
The TEM (Fig. 3d) image shows the presence of sub-10 nm
InSb NCs. Fig. 3e denotes a representative single InSb particle.
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Conclusion
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Colloidal InSb NCs were prepared by using commercially avail-
able InCl3 and Sb[NMe2]3 as In and Sb sources respectively.
The presence of a strong base such as LiN(SiMe3)2 or nBuLi or
LiBHEt3 was crucial for obtaining highly crystalline InSb NCs
as well controlling the size of the particle. The role of the base
is to convert InCl3 into more reactive In–C or In–N species via
an in situ salt metathesis reaction. This approach offers a
single pot method to generate InSb NCs using commercially
available reagents and avoids the use of sensitive organometal-
lic indium precursors or cumbersomely synthesized silyl-
amides. Various other potential bases and reducing agents,
solvent systems, and reaction conditions could be further
investigated to achieve greater control over size and shape of
the IR active InSb NCs.
Acknowledgements
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This work was supported by the Global Frontier R&D program
by the Center for Multiscale Energy Systems (2011-0031566)
and the Global R&D program (1415134409). ST acknowledges
Sikkim University for sanctioning study leave to carry out this
research work in Korea.
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