alpha-Zirconium phosphate (alpha-ZrP) was prepared by liquid-phase deposition. Boric acid was added to a solution containing [ZrF6](2-) anions, and phosphoric acid dropwise to cause slow decomposition of [ZrF6](2-) and the subsequent reaction with H3PO4 to form alpha-ZrP. X-ray diffraction, scanning electron microscopy, solid-state P-31 nuclear magnetic resonance spectroscopy, infrared spectroscopy, thermogravimetry, and elemental analyses indicate the formation of single-phase alpha-ZrP.