Currently, two approaches
dominate the large-scale production
of
MoS
2
: liquid-phase exfoliation, referred to as the top-down
approach, and bottom-up colloidal synthesis from molecular precursors.
Known colloidal synthesis approaches utilize toxic precursors. Here,
an alternative green route for the bottom-up synthesis of MoS
2
nanoflakes (NFs) is described. The NFs were synthesized by
colloidal synthesis using [Mo(CH
3
COO)
2
]
2
and a series of sulfur (S)-precursors including thioacetamide
(TAA), 3-mercaptopropionic acid (3-MPA),
l
-cysteine (L-CYS),
mercaptosuccinic acid (MSA), 11-mercaptoundecanoic acid (MUA), 1-dodecanethiol
(DDTH), and di-
tert
-butyl disulfide (DTBD). While
TAA, an S-precursor most commonly used for MoS
2
NF preparation,
is a known carcinogen, the other investigated S-precursors have low
or no known toxicity. High-resolution scanning transmission electron
microscopy (HR-STEM) and grazing incidence wide-angle X-ray scattering
(GIWAXS) confirmed that in all cases, the syntheses yielded single-layer
MoS
2
NFs with lateral sizes smaller than 15 nm and a well-defined
crystal structure. Electronic absorption and Raman spectra showed
characteristic features associated with the MoS
2
monolayers.
The evolution of the absorption spectra of the growth solution during
the syntheses reveals how the kinetics of the NF formation is affected
by the S-precursor as well as the nature of the coordinating ligands.