Abstract: | We have measured the time evolution of the self‐assembly process in perpendicular‐oriented cylindrical‐phase diblock copolymer thin films using statistical analysis of high‐resolution scanning electron microscope (SEM) images. Within minutes of annealing above the polymer glass‐transition temperature, microphase separation between polymer blocks results in formation of uniform nanometer‐scale domains whose relative position is initially largely uncorrelated. On further annealing, the cylindrical polymer domains organize into a two‐dimensional hexagonal lattice whose characteristic grain size increases slowly with time (~t1/4). © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 1970–1975, 2004 |