The acrylamide assisted polymeric citrate route was investigated for the synthesis of nanocrystalline ZrO2 powders, using zirconium oxychloride as the source for metal ion along with citric acid and acrylamide as chelating as well as polymerizing agents. The complete process for the synthesis of nanocrystalline ZrO2 powders was monitored by TG/DTA, FTIR, XRD and TEM techniques. Thermal decomposition of the polymeric intermediate was investigated using TG/DTA analysis. Structural coordination and phase of the synthesized ZrO2 powders were investigated by FTIR and XRD analysis respectively. The microstructure of the synthesized nanocrystalline ZrO2 powder was identified using transmission electron microscopy, which showed -lOnm agglomerates of still finer ZrO2 particles.