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We report on the near edge X-ray absorption fine structure (NEXAFS)spectroscopy of hybrid organic-inorganic resists. These materials arenonchemically amplified systems based on Si, Zr, and Ti oxides, synthesizedfrom organically modified precursors and transition metal alkoxides by asol-gel route and designed for ultraviolet, extreme ultraviolet and electronbeam lithography. The experiments were conducted using a scanning transmissionX-ray microscope (STXM) which combines high spatial-resolution microscopy andNEXAFS spectroscopy. The absorption spectra were collected in the proximity ofthe carbon edge (~ 290 eV) before and after in situ exposure, enabling themeasurement of a significant photo-induced degradation of the organic group(phenyl or methyl methacrylate, respectively), the degree of which depends onthe configuration of the ligand. Photo-induced degradation was more efficientin the resist synthesized with pendant phenyl substituents than it was in thecase of systems based on bridging phenyl groups. The degradation of the methylmethacrylate group was relatively efficient, with about half of the initialligands dissociated upon exposure. Our data reveal that the such dissociationcan produce different outcomes, depending on the structural configuration.While all the organic groups were expected to detach and desorb from the resistin their entirety, a sizeable amount of them remain and form undesiredbyproducts such as alkene chains. In the framework of the materials synthesisand engineering through specific building blocks, these results provide adeeper insight into the photochemistry of resists, in particular for extremeultraviolet lithography.

Changes in the near edge X-ray absorption fine structure of hybrid organic-inorganic resists upon exposure