The hardening behavior of precipitation was studied during aging of Fe-Cr alloys. This mechanical behavior is associated with the nanometric modulation structure of the coherent decomposed Fe-rich and Cr-rich phases formed by the spinodal decomposition of the supersaturated solid solution. The growth kinetics of spinodal decomposition was very slow and it increased during coarsening stage. The morphology of decomposed phases consisted of an interconnected irregular shape with no preferential alignment for short aging times and a further aging caused the change to a plate shape of the decomposed Cr-rich phase aligned in the <110> directions of the Fe-rich matrix. The rapid increase in hardness and embrittlement seem to be associated with the coherency and nanometer size of the spinodally-decomposed phases in the aged alloys.