Considerable research has been carried out on colloidal semiconductor nanocrystals (NCs) on account of their size dependent electronic and optical properties, which are the key issues in many applications, such as biomedical fluorophores, 1 LEDs, 2 and photovoltaic devices. 3 Among them, a group of II-VI semiconducting NCs, for example, CdSe quantum dots (QDs), exhibit excellent photostability, quan-tum yield (QY), and a tunable emission wavelength. 4,16 However, CdSe QDs have limited applications owing to their intrinsic toxicity. 5 It is believed that III-V QDs, particularly InP NCs, are the most desirable alternative. However, the photoluminescent quantum yield tends to be very low due to nonradiative surface recombination sites and high activation barriers for carrier detrapping. 6,7 A core-shell structure appears to be essential for surface passivation, but limited numbers have been reported, including InP/ZnS 8,9,14,15 and InP/ZnCdSe 10 core/shell QDs. HF etching 11,13 and low reaction temperature methods have also been attempted. In particular, the recent reports by Peng's group on highly luminescent InP/ZnS core-shell quantum dots in the visible range using fatty amine 9 and Reiss on the one-pot synthesis of InP/ZnS 14 are quite impressive.We report the stepwise synthesis of InP/ZnS core-shell quantum dots and the role of zinc acetate during the reaction. Zinc acetate was used as a precursor for zinc and acetic acid. Highly luminescent InP/Zn-palmitate was obtained as an intermediate. The InP core was synthesized with indium acetate (In(OAc) 3 ), tris(trimethylsilyl)phosphine ((TMS) 3 P), and palmitic acid as the indium and phosphorus precursors