Influence of high-pressure processing on the structure and memory effect of synthetic layered double hydroxides

We investigate the structural evolution of synthetic layered double hydroxides (LDH) samples, processed at room temperature and high-pressure (up to 7.7 GPa) in a toroidal chamber with two pressure-transmitting media, lead and graphite, using X-ray diffraction, thermogravimetry and N₂-adsorption isotherms techniques. The X-ray patterns of compacted samples show a decrease in the peak intensities. For both pressure-transmitting media, our samples revealed a reduction of the basal d-spacing for the (003) plane when processed at 7.7 GPa. The expected high-pressure-induced amorphization was not observed. Surprisingly, we find high-pressure processing to have a strong influence on the memory effect of the LDH, due essentially to the reduction of the surface area and pore closing. Even when immersed in water, our samples did not recover the LDH structure, when either calcined at 450°C and compacted at 7.7 GPa, or calcined at 700°C and immediately compacted at 2.5 and 7.7 GPa.