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Hydrogen-bonded polymer complex films with the thickness ranging from 50 nm to 2400 nm were prepared by layer-by-layer (LbL) assembly of poly(2-ethyl-2-oxazoline) (PEOX) and poly(acrylic acid) (PAA). The dewetting behavior of PEOX/PAA films under hydrothermal condition was investigated. It was found that the dewetting occurred at solid-liquid interface, and the typical morphologies such as holes, irregular cellular structure, and droplets were observed. Atomic force microscopy (AFM) revealed the initial rupture of the film. Microscopic Raman and infrared (IR) imaging demonstrated that the PEOX and PAA chains remained association during the dewetting process. [ABSTRACT FROM AUTHOR]