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The molecular configuration and chemistry at the zinc/zinc oxide−polyester interface were studied by using two complementary spectroscopic techniques: attenuated total reflection−Fourier transform infrared spectroscopy (ATR-FTIR) and sum-frequency generation (SFG) spectroscopy. It was shown that ATR-FTIR should be considered as a (3D) interphase-sensitive technique with probing depths of 250−400 nm in the headgroup region (2000−1200 cm −1 ). On the other hand, SFG is known to be a (2D) interface-sensitive technique. The ATR-FTIR measurements showed that carboxylate groups are formed within the nearinterface region of the polyester phase. SFG measurements showed that the carboxylic acid groups are stable at the polymer−zinc/ zinc oxide interface. In addition, in situ ATR-FTIR and SFG measurements have been conducted when exposing the polyester− zinc/zinc oxide system to D 2 O. The exposure to D 2 O is observed to lead to an additional conversion of ester and carboxylic acid groups to carboxylate groups. The comparison of the SFG and ATR-FTIR measurements shows that this conversion occurs much slower at the polyester−zinc/zinc oxide interface than in the bulk of the polyester. Finally, the strengths and limitations as well as the complementarity of both techniques are discussed.

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