Mapping the oxygen structure of γ-Al2O3 by high-field solid-state NMR spectroscopy

γ-Al 2 O 3 is one of the most widely used catalysts or catalyst supports in numerous industrial catalytic processes. Understanding the structure of γ-Al 2 O 3 is essential to tuning its physicochemical property, which still remains a great challenge. We report a strategy for the observation and determination of oxygen structure of γ-Al 2 O 3 by using two-dimensional (2D) solid-state NMR spectroscopy at high field. 2D 17 O double-quantum single-quantum homonuclear correlation NMR experiment is conducted at an ultra-high magnetic field of 35.2 T to reveal the spatial proximities between different oxygen species from the bulk to surface. Furthermore, 2D proton-detected 1 H- 17 O heteronuclear correlation NMR experiments allow for a rapid identification and differentiation of surface hydroxyl groups and (sub-)surface oxygen species. Our experimental results demonstrate a non-random distribution of oxygen species in γ-Al 2 O 3 . γ-Al 2 O 3 is widely used in catalytic processes, but understanding its detailed structure remains a challenge. The authors, using two-dimensional solid-state NMR spectroscopy at a high magnetic field, characterize the spatial proximity and connectivity between oxygen species from the bulk to the surface.