We report the observation of a reversible thermotropic transition betw
een the lamellar and cylindrical morphologies in a polystyrene-poly(et
hene-co-butene) diblock copolymer. The nature of the intermediate stru
ctures which form as the transition progresses has been examined using
two-dimensional small-angle X-ray scattering (SAXS) and transmission
electron microscopy (TEM). Results show that the transformation from t
he lamellar to the cylindrical morphology proceeds in two steps. Initi
ally, fluctuations along the interface joining the components of the c
opolymer grow in amplitude until the lamella transforms into a sheet o
f evenly spaced cylinders; cylinders which form in adjacent lamellae a
re usually in poor register with one another. This intermediate struct
ure subsequently anneals into the hexagonal packing of cylinders chara
cteristic of the cylindrical morphology. The reverse transition from c
ylinders to lamellae proceeds without producing any intermediate signa
ture detectable by SAXS.