Synthesis and Structural Analysis of Ternary Ca–Al–Fe Layered Double Hydroxides with Different Iron Contents

Hydrocalumite structured layered double hydroxides (LDHs) with various Fe3+ ratios were prepared through a coprecipitation method. In order to control the Fe3+ content in LDH, binary Ca–Fe LDHs were first synthesized with various Ca/Fe ratios. The X-ray diffraction pattern showed that only a limited Ca/Fe ratio resulted in LDH formation. The Fe3+ content in LDH was controlled by applying Al3+ while the divalent and trivalent metal ratio was set to 2. Through X-ray diffraction patterns, ternary LDHs with Ca–Al–Fe composition were successfully synthesized without significant impurities, with the Al increasing crystallinity. Quantification showed that Al moiety participated in the formation of the LDH framework more than Ca and Fe, implying a structural stabilization in the presence of Al. In order to investigate the global and local structure of Fe moiety in the LDH, both solid state UV-vis and X-ray absorption spectroscopies were carried out. Both spectroscopies revealed that the existence of Al induced slight local distortion in coordination but global crystal stabilization.