Synthesis of La2Ti2O7 nanoscale powder and ceramics based on it by sol-gel and spark plasma sintering

The application of ceramics as matrices for the immobilization of radionuclides for the purpose of their safe long-term disposal or beneficial use is being studied with an emphasis on phase stability, structural integrity, hydrolytic stability, etc. In this work, a combined approach was investigated, based on the sol-gel citrate synthesis of nanosized La2Ti2O7 powder and its subsequent spark plasma sintering to produce dense ceramics. The phase composition and structure of the nanosized La2Ti2O7 powder and ceramic samples based on it, obtained in the temperature range of 900–1300 °C, were studied by XRD and SEM. It has been shown that the powder synthesis conditions ensure the formation of nanosized crystalline La2Ti2O7 grains, whose consolidation under spark plasma heating conditions proceeds with a change in the phase composition from single-phase La2Ti2O7 of monoclinic structure to orthorhombic with an admixture of LaTiO3 at temperatures above 1200 °C. It was revealed that the change in the ceramic structure is accompanied by the formation of non-porous and defect-free monolithic samples. It was determined that such a change leads to an increase in relative density (81.3–95.7%) and compressive strength (78–566 MPa) of the ceramic samples. However, the hydrolytic stability of the ceramics decreases, as indicated by an increase in the leaching rate of La3+ from 10–7 to 10–5 g/cm2·day. The obtained results are useful for the systematic study of materials suitable for immobilization technologies of radioactive waste in ceramics.