Structure of Layered Double Hydroxides and the reaction occurring duri
ng thermal treatments are investigated. The reaction is supposed to be
a grafting reaction of interlamellar species onto layers but its mech
anism is not well known. These materials display a very poor level of
organisation and the study of their fine structure involves the use of
techniques sensitive to the local environments. XANES and EXAFS studi
es give few information about the grafting process because of the grea
t disorder in the interlayer space. Much more information about the la
yers local structure are reached, revealing that distorted and regular
octahedra coexist which is particular to layers containing copper ato
ms. It probably creates a local segregation undetectable by X ray diff
raction study in anyway. Tt also highlights the difference of sheet th
ermal stability in function of the nature of the intercalated anion.