Blends A/alphabeta and C/alphabeta of a polymer A or C and a diblock c
opolymer alphabeta with blocks alpha and beta of equal lengths were an
alyzed, where A is chemically equal to a while C has attractive intera
ctions with alpha. Films of the blends were cast, using nonselective s
olvents. The random phase approximation model predicts a transition fr
om microscale to macroscale fluctuations in the still homogeneous solu
tions, the transition depending on the chain lengths of A or C, relati
ve to that of alphabeta, on the interactions, in particular those of C
and a, and on the temperature. This transition was observed, where pr
edicted, in cast films of various blends of a diblock copolymer P(MMA-
b-S) of methyl methacrylate and styrene. The microphase and macrophase
morphologies of blends with PMMA as well as PS, SAN, poly(cyclohexyl
methacrylate), and tetramethyl polycarbonate were characterized by ele
ctron microscopy. Effects that are not predicted by the model are show
n to come from secondary segregation processes. Quite a variety of mor
phologies can be produced.