Nanocrystalline ZrO2 powders have been prepared using acrylamide assisted polymeric citrate combustion (autoignition) route. Process parameters (i.e., total metal ions to citric acid ratio) were varied for the formation of polymeric resin in order to obtain the final product with desired properties (organic free, smaller crystallite size, etc.). The effect of three different citric acid amounts in the formation of nanocrystalline ZrO2 powder was investigated using FTIR, XRD, TG/DTA and SEM-EDS, respectively, to identify the structural coordination, phase, thermal behavior and microstructure of the polymeric intermediates as well as the final ZrO2 powders. Organic free ZrO2 powder with two different phases of metastable t-ZrO2 and m-ZrO2 were prepared by calcining the polymeric intermediates at 600 degrees C. The lowest crystallite was found to be 18 and 16 nm, respectively, for the t-ZrO2 and m-ZrO2 phases prepared with total metal ions to citric acid ratio of 1:3. (C) 2009 Elsevier B.V. All rights reserved.