117
Mater. Res. Soc. Symp. Proc. Vol. 1493 © 2013 Materials Research Society
DOI: 1 557/op 013 0.1 l.2 .4
Passivation, Separation and Characterization of Plasma Synthesized Silicon Nanoparticles
Jifang Cheng
1
, Catherine Jimenez
1
, Jacob P. Bell
1
, Ingrid E. Anderson
2
, Chito Kendrick
2
,
Yongan Yang
1
, Reuben T. Collins
2
and S. Kim R. Williams
1
1
Chemistry and Geochemistry Department, Colorado School of Mines,
1500 Illinois St, Golden, CO 80401, U.S.A.
2
Physics Department, Colorado School of Mines,
1500 Illinois St, Golden, CO 80401, U.S.A.
ABSTRACT
Silicon nanoparticles (Si NPs) were synthesized by plasma enhanced chemical vapor
deposition (PECVD) using silane as a silicon source. Allylamine was used as passivation ligands
to form water-soluble Si NPs. Finally, aqueous asymmetric flow field-flow fractionation was
used to successfully separate the polydisperse Si NPs into monodisperse Si NP fractions.
INTRODUCTION
Semiconductor nanoparticles with unique optical and electronic properties have shown
potential application in many fields from sensor technology to optoelectronics
[1-3]
. With their
tunable band-gap
[4,5]
, low toxicity, and biocompatibility
[6-8]
, silicon nanoparticles (Si NPs) have
generated wide interest among scientists in various research areas. Important properties of these
nanoparticles such as photoluminescence, absolute quantum yields, and exciton lifetime are size-
dependent
[4,9,10]
. Significant research effort has been directed towards controlled synthesis of
monodispersed Si NPs with desirable properties. However, most synthesis procedures yield
polydispersed Si NPs with significant size inhomogeneity. Thus, the need for development of
post-synthesis, purification and separation methods has become a necessity, albeit one that has
not yet received a great deal of attention. Gradient density ultracentrifugation
[10]
and size-
selective precipitation
[9]
have been reported as successful approaches for post synthesis size-
separation of Si NPs. In this work, aqueous asymmetric flow field-flow fractionation (AF4) was
used to separate Si NPs into homogenous fractions with narrow size distributions.
EXPERIMENT
Si NPs with small diameters were synthesized by PECVD at a pressure of ~4x10
-3
Torr
with 13.56 MHz radio frequency at 40 Watt plasma. The feed gas was 1.4 sccm of SiH
4
heavily
diluted in 275 sccm of argon. The as-synthesized Si NPs were etched in 5% HF for about 5
minutes to remove dangling bonds and obtain hydrogen terminated Si NPs. These hydrogen-
terminated Si NPs were passivated by allylamine under hydrogen hexachloroplatinate (IV)
(H
2
PtCl
6
) as the catalyst in isopropanol. The allylamine-terminated Si NPs were separated by
aqueous AF4 using 0.001% FL-70 in distilled ion (DI) water as a carrier liquid with a ultraviolet
(UV) detector to identify the sample elution information. The allylamine-terminated Si NPs and
blue dye were focused on narrow bands at about 2 mm intervals, which were 3.4 cm from the
inlet, and 24.6 cm from the outlet. Different fractions containing monodispersed Si NPs were
04