By using a simple and efficient deuteration process, (2)H has been successfully introduced into layered double hydroxides (LDHs). Due to significantly less (1)H-(1)H homonuclear dipolar coupling, high-resolution (1)H solid-state NMR spectra can now be obtained conveniently at medium to low spinning speed to extract the information of cation ordering in LDHs. Furthermore, we show that double-resonance experiments can be applied easily to investigate internuclear proximities and test possible cation-ordered superstructure models. This approach can be readily extended to LDHs with different compositions to explore the local structure and the key interactions between the cations in the layer and interlayer anions.
Keywords: 2H; LDH; MAS NMR; cation ordering; high resolution.