Nanocrystals of zinc oxide (ZnO) were prepared from diethylzinc and donor-functionalized alcohols, 2-methoxyethanol, 2-ethoxyethanol, and 2-methoxyethoxyethanol by sol-gel processing. The nanocrystals were prepared at room temperature and characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED). Crystal sizes were controlled by the type of utilized donor-functionalized alcohol in which decreased by an increase of the chain length and type of the donor-functionalized alcohol from 16 to 27nm. The HRTEM and SAED results revealed that the degree of crystallinity decreases with increasing donor-functionalized alcohol chain length. The particle size of the ZnO powders demonstrated high tolerance to heat treatment and grow up to approximately 65 to 80nm upon calcination at 1000°C.