A composition of zirconyl hydroxy chloride and aluminum chlorhydroxide in stable solid form having improved antiperspirant efficacy when dissolved in water is made by heating a 2-20% by weight aqueous solution containing at least the aluminum chlorhydroxide component of the composition at a temperature of at least 50.degree. C. until the ratio of the height of peak 4 at Kd=0.7 to that of peak 3 at Kd=0.5 as measured by gel permeation chromatography on cross-linked dextran is at least 2:1, then subjecting the solution to rapid drying to solid form.