Mono-dispersed sub-micron sized hydrotalcite-like compounds (HTlcs), [Mg_1−xAl_x(OH)₂](CO₃)_y·2H₂O, were synthesized by the urea hydrolysis method. The as-prepared compounds display platelet-like primary particles with a hexagonal shape. The breadth to thickness ratio can be varied by changing the synthesis conditions such as the precipitation rate or the medium nature. The factors influencing the secondary particle morphology (or aggregates) are also discussed. The results are compared to the constant pH coprecipitation method, commonly used for HTlcs.

Delamination of the layered double hydroxide structure [Zn₂Al(OH)₆][C₁₂H₂₅SO₄ ·nH₂O] was realized by dispersion in butanol; translucent colloidal solutions are stable for at least 8 months with oriented LDH materials with extended crystallite size being obtained; the results presented here suggest that total delamination occurs in the colloidal solution.

Layered double hydroxides recovered after exfoliation have been characterized by solid state chemistry techniques. The nature of the recovered materials is highly dependant on the drying process; when gently dried, a well-ordered phase is obtained, either by freeze-drying or reconstruction, but the material becomes amorphous after evaporation of the solvent. Delamination was used to prepare interstratified LDHs, making this technique a new route to the formation of a wide range of tunable materials.