Phosphogypsum is the by-product of phosphate of fertilizer or phosphate which causes serious environmental pollution. In this work, a series of phosphogypsum whiskers were prepared using phosphogypsum as raw materials and NH 4 Cl as additive through the atmospheric water solution method. The results showed that the ammonium chloride solution has a great influence on phosphogypsum whiskers growth and the solubility. The best whisker aspect ratio of phosphogypsum was preferred in 1 mol/L NH 4 Cl solution, in which the solubility achieved 6.434 mg/mL and the aspect ratio reached 69.29. Besides, NH 4 Cl was found to have a modified effect on gypsum whiskers' growth and it can be used to get mesh or dendritic whiskers.