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Porous magnesium-aluminium layered double hydroxides (LDH) were prepared through intercalation and decomposition of hydrogen peroxide (H 2 O 2 ). This process generates oxygen gas nano-bubbles that pierce holes in the layered structure of the material by local pressure build-up. The decomposition of the peroxide can be triggered by microwave radiation or chemically by reaction with iodide (I − ) ions. The carbonate LDH version [Mg 0.80 Al 0.20 (OH) 2 ](CO 3 ) 0.1 ∙mH 2 O was synthesized by microwave-assisted urea coprecipitation and further modified by iodide or H 2 O 2  intercalation. High resolution Scanning Electron Microscopy (HR-SEM) and Brunauer-Emmet-Teller (BET) analysis were used to assess the morphology and surface area of the new porous materials. The presence of H 2 O 2  in the interlayer region and later decomposition triggered by microwave radiation generated more pores on the surface of the LDH platelets, increasing their specific surface area from initially 9 m 2 /g to a maximum of 67 m 2 /g. X-Ray Diffraction showed that the formation of the pores did not affect the remaining crystal structure, allowing possible further functionalization of the material.

Porous Layered Double Hydroxides Synthesized using Oxygen Generated by Decomposition of Hydrogen Peroxide