A soft-contact film transfer method was developed to prepare multilayer photoresist thin films that enable high-resolution spectroscopic and reflectivity measurements for determining the reaction−diffusion kinetic parameters and photoacid diffusion length. Infrared reflectance absorption spectroscopy was applied to follow, quantitatively, the reaction−diffusion kinetics during the post-exposure bake (PEB) step; the time evolution of the average deprotection level across a bilayer film with model photoresists is described by a kinetics model with three parameters: a reaction rate constant (kP), the phenomenological photoacid trapping constant (kT), and the photoacid diffusion constant (DH). A polymeric and molecular resist for next-generation extreme ultraviolet (EUV) lithography with chemically analogous structure was studied with this methodology. The three kinetic parameters follow an Arrhenius dependence but show quantitative differences between these two photoresists at a given PEB temperature. Furthe...