In order to investigate solid state phase transformation in solid, Nd1-xBa2
-xCu3O6+delta powders with different compositions were annealed under diffe
rent annealing conditions. The temperature-substitution ratio-oxygen conten
t phase diagram of Nd1+xBa2-xCu3O6+delta solid solution was constructed. Th
e condition to occur Nd123ss phase separation was clarified by investigatin
g the compositional fluctuation, XRD pattern, the time dependences of T-c p
roperties and oxygen content. Solid state phase transformation of Nd123ss a
dvances with two steps. Tetragonal orthorhombic phase transition due to oxy
gen introduction occurs at first, and then the orthorhombic phase with smal
l x decomposes to the two phases by spinodal decomposition.