The QDs can be synthesized with Schlenk-line at high
temperature.A traditional synthesis CdSe QDs procedure is to use organic
compounds,such as TOPO, Dimethylcadnium(DMC), TOP and Selenium under
high temperature and Argon protection to react.
The QDs we got by use of the approch is coated
with organic compounds (TOPO, HDA, ODA etc.) Only can be dissolved
in organic solvent ( Hexanes, Chloroform, THF, Pyridine, Toluene etc.)and
has High Quantum Yield(>40%)
In order to improve the quantum yield of the QDs
and protect QDs from photooxide, the core-shell structure is used
to synthesize the Qds. As a shell, ZnS can increase the band gap of
the QDs so that the quantum yield can be raised to 80%.
As ligands, TOPO and HDA or ODA often be used to
synthesis high quality quantum dots. the synthesis mechanism shows
that HDA or ODA can improve the size distribution of the nanoparticlized
form process and increase QDs quantum yield because of amine group
action.
The Schlenk line ¨C 6-knob vacuum manifold,Fume hood,
Glove box, Auto-temperature controllable heater,UV-Vis spectrophotometer
and Spectrofluorometer are basic equipments and devices for the synthesis.
Tip1:
As a standard, the properties of high
quality QDs should be
Quantum Yield >40%-80%;FWHM<30nm;Photo-oxcided
resistance.
Tip2:
A protocol for QDs synthesis ( 550nm-640nm)
TOPO(90%) 8g, HDA(90%) 5g, DMC 0.2mmol, TOPSe soluton(1M)
4ml.
TOPO and HDA were put in 150ml three neck flask to
degas for 30min at 150°C under stirring. Then add 0.2mmol DMC
to continue degas for 15min.Afterwards,the argon was refilled into
flask and the temperature was raised to 300°C. At this temperature
point, the 4ml TOPSe was injected into flask rapidly. The temperature
was kept at 280°C for QDs growth(the solution color was changed
from yellow to dark).The sample was picked up at different time(from
30s to 4min). The different of color QDs can be got.At 270°C,
add ZnS TOP solution 1-3ml for capping and cool down temperature rapidly.