Probing porosity and pore interconnectivity in crystalline mesoporous TiO ₂ using Hyperpolarized ¹²⁹Xe NMR

Hyperpolarized (HP) ¹²⁹Xe NMR was used to probe the porosity and interconnectivity of pores in crystalline mesoporous TiO ₂. We have demonstrated that HP 129Xe NMR can be used to differentiate between similar sized pores within different crystalline phases. Pores of 4 nm size resident in mixed anatase and rutile mesoporous TiO ₂ phases were identified. Complementary to other pore characterization techniques, HP ¹²⁹Xe NMR is able to probe the interconnectivity between pores present in these different phases. The cross peaks in 2D exchange (EXSY) NMR spectra between the signals of xenon in two types of pores are visible on millisecond timescale, indicating substantial pore interconnectivity. The obtained information on porosity and interconnectivity is important for the understanding of ion transport mechanisms in mesoporous TiO ₂ anode materials.