Two types of (Zn, Al) layered double hydroxide were prepared by a hydrothermal process at room temperature using Zn salt precursors on Al foils. The examined LDHs differ for the hosted anions in the interlamellar space, namely Cl À and NO 3 À . Scanning electron microscopy, X-ray photoelectron spectroscopy and ultraviolet photoemission spectroscopy have been used to characterize four types of the samples, representative of the two hosted anions (Cl À and NO 3 À ) and two times of growth (6 and 24 h). X-ray photoelectron spectroscopy results permitted to describe the interactions between inorganic anions hosted in the interlamellar space and the metallic cations on the brucite layer. They also allowed giving a tentative explanation of the different morphologies observed by scanning electron microscopy.