Effects of ultrasonic irradiation on the synthesis, crystallization, thermal and dissolution behaviour of chloride-intercalated, co-precipitated CaFe-layered double hydroxide.

• Mapping the influence of ultrasound irradiation on co-precipitated CaFe-Cl−-LDHs. • Continuous irradiation resulted in elevated crystal thickness and anion incorporation capacity. • On pulsed irradiation, porosity was developed and the aggregate size was reduced. • Detailed thermal, dissolution and optical description of sonocrystallized LDHs was given. • The integrity of the interlayer structure was preserved up to 200 °C. The output power (30–150 W) and the periodicity (20–100%) of ultrasound emission were varied in a wide range to regulate and improve the crystallization process in the commonly used co-precipitation technique of chloride-intercalated CaFe-layered double hydroxides. The influence of ultrasound irradiation on the as-prepared materials was studied by X-ray diffractometry, dynamic light scattering, UV–Vis–NIR diffuse reflectance spectroscopy, specific surface area measurement, pore size analysis, ion-selective electrode potentiometric investigations and thermogravimetry. Additionally, structural alterations due to heat treatment at various temperatures were followed in detail by Fourier-transform infrared and X-ray absorption spectroscopies as well as scanning electron microscopy. The ultrasonic treatment was capable of controlling the sizes of primarily formed (from 19 nm to 30 nm) as well as the aggregated (secondary) particles (between 450 nm and 700 nm), and thus modifying their textural parameters and enhancing the incorporation of chloride anions into the interlamellar space. For the first time, the optical energy gap of CaFe-LDH was reported here depending on the nature of applied stirring (4.18–4.34 eV). The heat-treatment investigations revealed that the layered structure was stabile until 200 °C, even at the atomic level. [ABSTRACT FROM AUTHOR]