Zinc hydroxide nitrate, a brucite-like layered material was synthesized using pH control method. Poly(vinyl alcohol) and poly(ethylene glycol) were used at various percentages as size decreasing agents during the synthesis of zinc hydroxide nitrate. SEM and PXRD showed the decrease of size and thickness of the resultant zinc hydroxide nitrates. TG and surface area data confirmed the decrease of the particle sizes, too. When zinc hydroxide nitrates were heat treated at 500 °C, the physical properties of nano zinc oxides obtained depended on the parent material, zinc hydroxide nitrate.