Crystallization and melting of a poly(ethylene oxide) (PEO) diblock copolymer containing a tablet-like block of poly {2,5-bis[(4-methoxyphenyl)oxycarbonyl] styrene} (PMPCS) in ultrathin films have been studied using atomic force microscopy (AFM) coupled with a hot stage. The PEO and PMPCS block possess the number-average molecular weights (M-n) of 5300 and 2 100 g/mol, respectively. The ultrathin films on the mica and glow-discharged carbon surfaces were obtained by static dilute solution casting at room temperature. Isothermal melt crystallization from ultrathin films always leads to flat-on lamellae. Selective area electron diffraction (SAED) experiments have demonstrated that the PEO blocks crystallize with a monoclinic structure identic...