Many types of metal oxide nanocrystals (NCs) and nanoparticles (NPs) as high-energy-density anode materials have been limited by their ionic and electronic conductivities and can withstand much larger volumetric …show more content…
4-iodobenzoic acid in DMF (IBA, 0.05 g, 98%, Sigma-Aldrich; in 5 mL) was ligand-exchanged with In2O3 NC-OA in hexane (0.1 g in 10 mL). The In2O3 NC-IBA can dissolve well in DMF. The room temperature Sonogashira coupling reaction of 4,4′-(ethyne-1,2-diyl)dibenzoic acid capped In2O3 NC (In2O3 NC-EBA) was prepared as follows: a 100 mL round flask with a stirring bar was fitted with a rubber septum and flame dried under vacuum. The flask was purged with dry argon and charged with 0.2 g of starting material In2O3 NC-IBA in 6 mL of anhydrous DMF (yellow transparent solution). In addition, Pd catalyst (PdCl2(PPh3)2, 20 mg, 98%, Sigma-Aldrich) and CuI (20 mg, 98%, Sigma-Aldrich) was sequentially added. Septum was parafilmed after the discharge of solids. Argon-spraged 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU, 852 µL, 98%, Sigma-Aldrich) was then added by a syringe. Ice-chilled ethynyltrimethylsilane (100 µL, 98%, Sigma-Aldrich) was loaded, followed immediately by distilled water (40 µL). The reaction flask was covered with an aluminum foil and left stirring at high rate of speed for 24 h. At the end of the reaction, the dark powder was aggregated at the bottom of the flask. The collected powder was washed with bi-solvent of ethyl ether and distilled water-DI (10 mL each), followed by washing step with 10% HCl, saturated aqueous