Amorphous zinc phosphate nanospheres were prepared via a sonochemical route. Zinc phosphate nanospheres were uniform in shape with an average diameter of 210 nm. The average diameter of nanospheres could be controlled by changing the pH of a precursor solution. This sonochemical method is simple, facile, economical, and environmentally benign. Non-crystalline characteristics of as-prepared zinc phosphate nanospheres were confirmed by X-ray diffraction, transmission electron microscopy, and FT-IR spectroscopy analyses. We believe this technique will be readily adopted in realizing other forms of zinc phosphate nanostructures.