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Layered double hydroxides (LDH) and layered hydroxide salts (LHS) are widely studied as matrices to design new materials with applications in several areas of science and technology. Both LDH and LHS are composed of molecular layered units with surfaces fully covered by hydroxyl groups and positive‐charge residues within the layers; therefore, anions in the interlayer space are needed. Even though these anions are described as interlayer species without a covalent interaction with the molecular layered units, the substitution of hydroxyl groups is also possible; in other words, the functionalization of the surface could occur. This chapter reviews results previously published related to the functionalization phenomenon in LDH and LHS, which is not considered in most of the scientific reports of new materials derived from these compounds. In this text, the use of copper probes to study electron paramagnetic resonance spectra, reinforced with infrared spectroscopy to confirm functionalization, is described. The occurrence of functionalization instead of a simple anion exchange provides a change of properties in the final nanosized material.

Functionalization of Surfaces in Layered Double Hydroxides and Hydroxide Salt Nanoparticles