In order to investigate phase separation in solid, Nd1+xBa2-xCu3O6+delta po
wders with different compositions were annealed under different annealing c
onditions. The temperature - substitution ratio - oxygen content phase diag
ram of Nd1+xBa2-xCu3O6+delta solid solution (Nd123ss) was constructed. The
condition to occur Nd123ss phase separation was clarified by investigating
the compositional fluctuation, XRD pattern, the time dependences of T-c pro
perties and oxygen content. Consequently, only orthorhombic phase with smal
l x can separate into two orthorhombic phases with larger and smaller x by
the spinodal decomposition mechanism. (C) 2001 Elsevier Science B.V. All ri
ghts reserved.