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TEM and selected area electron diffraction (SAED) were performed using a JEOL 2010F TEM operating at 200 kV equipped with a GATAN digital photography system. TEM samples were prepared by drop casting nanocrystals from chloroform dispersions onto 200 mesh copper grids with ultrathin carbon film (Ladd Research, VT) or lacy carbon film (Electron Microscopy Sciences, PA). Energy-dispersive X-ray spectroscopy (EDS) was performed on the JEOL 2010F HRTEM equipped with an Oxford spectrometer.
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2642540359
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The Ge precursor solution was loaded into a 1 mL titanium grade-2 cell (0.5 cm i.d., 2.0 cm o.d., and 7.0 cm long with a titanium grade-2 LM6 HIP gland and plug, High-Pressure Equipment, Inc) in a nitrogen glovebox. A brass block (7 x 25 x 17 cm) was used to heat the reactor. The block was thermostated with a thermocouple (Omega, Inc.) and a temperature controller, and heated by four 300 W 1/4 in. diameter by 4.5 in. long cartridge heaters (Omega). The block was heated to the desired reaction temperature prior to inserting the cell. The cell was inserted into the preheated block and reached the synthesis temperature in 2 min. The reaction proceeded another 5 min for TEG and 20 s for DPG at this temperature.
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