Neodymium zirconyl oxalate (NdZrOX) is prepared and characterized by chemical analysis and ir spectral studies. Its thermal decomposition has been investigated by using DTA, TG, DTG, X-ray diffraction and ir spectroscopy. On the basis of thermogravimetry and isothermal studies a probable mechanism for the decomposition is proposed. The decomposition proceeds mainly through three stages: i) dehydration between RT-413 K, ii) decompodtion of oxalate between 413-943 K and iii) decomposition of the carbonate between 1028--1235 K to give a mixed oxide. The ir spectra and X-ray diffraction studies are made for identification of the intermediates. X-ray diffraction studies of the end product indicates that it belongs to cubic crystal system with a = 11.520 A.In recent times the quest for high purity ceramic materials of controlled particle size, particularly for electronic industry, has led the chemists to search for different techniques for the preparation of various mixed oxide ceramics. It has been demonstrated by several workers that high purity titanates, stannates, ferrites, zirconates of perfect stoichiometry can be prepared from pyrolysis of mixed metal oxalate systems [1][2][3][4]. Zirconium is reported zo form anionic oxalato zirconates [5] and thermal decomposition of such complex s~lts make up an interesting study. The lack of literature on oxalato zirconates of trivalent cations led us to prepare and study the thermal decomposition of neodymium zirconyl oxalate whose end product is expected to be a mixed oxide.