Photovoltaic Devices Employing Ternary PbSxSe1-x Nanocrystals Page: 3 of 18
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successfully obtained monodisperse, highly crystalline nanocrystals using a one-pot, hot
injection synthesis. Lead oxide (PbO, 99.999%), selenium (99.99%), oleic acid (OA,
tech. grade, 90%), diphenylphosphine (DPP, 98%), 1,3-benzenedithiol (BDT, >98%),
bis(trimethylsilyl) sulfide (TMS2S, purum), 1-octadecene (ODE, 90%), anhydrous
solvents and aluminum shot (99.999%) were purchased from Aldrich and used as
received. Trioctylphosphine (TOP, >97%) was acquired from Strem. Nanocrystal
synthesis was performed under argon atmosphere using standard air-free Schlenk line
techniques. The synthesis scheme is as follows: A solution of 446mg PbO (2 mmol), 1.4
g oleic acid (5 mmol), and 10 g ODE was degassed and heated to 150 C in a 50 mL
three-neck flask for one hour. A mixture of proper amount 1M TOP:Se solution, TMS2S,
DPP (40mg) and ODE was then rapidly injected into this hot solution. The Se and S
precursor ratio was tuned to specific values, but the total amount was kept at 1 mmol.
ODE was added to dilute the precursor solution to 2 ml total. The nanocrystals were
grown at 150 C for 90 s, and the reaction was rapidly quenched by placing the flask in a
room-temperature water bath and injecting 5 mL of anhydrous hexane. The nanocrystals
were purified by precipitation twice in hexane/ethanol and once in hexane/acetone and
stored in a glovebox.
Achieving and characterizing a uniformly alloyed nanocrystal remains difficult.16
Complications arise from the difference in precursor solubility and reactivity at a given
temperature, and in the difference between nucleation and growth of nanocrystals. Since
TMS2S is more reactive than TOP:Se, the stoichiometric ratio of S to Se in the resulting
nanocrystal sample was greater than the injected precursor ratio. The composition of the
resulting nanocrystals was characterized using energy filtered transmission electron
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Ma, Wanli; Luther, Joseph; Zheng, Haimei; Wu, Yue & Alivisatos, A. Paul. Photovoltaic Devices Employing Ternary PbSxSe1-x Nanocrystals, article, February 5, 2009; Berkeley, California. (digital.library.unt.edu/ark:/67531/metadc933485/m1/3/: accessed November 19, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.