The oxygen deficient neodymium nickel perovskite, NdNiO3-x, has been o
btained by different low temperature-low oxygen pressure synthetic pro
cedures. Besides a solid-matrix based route, both ordered and disorder
ed chemical-precursors have been used as starting products. X-ray powd
er diffraction shows that the structure of this defective perovskite i
s orthorhombic. The study of the grain morphology of the products as r
esulting from the different synthetic procedures indicates that the ma
in parameter determining the average panicle size, which is in the nan
ometer range, is the maximum temperature achieved in the synthesis. Re
sistivity and DSC measurements show the existence of a metal to insula
tor transition at ca. 175 K. The anomalous behaviour of the resistivit
y in the insulator zone is discussed.