A2Zr2O7 (A=La/Gd/Yb): Grain growth effect on phase stability properties at 1300°C

The present study aims to investigate the influence of grain growth during heat treatment on the phase stability of AZO: A2Zr2O7 compounds at 1300°C. To this end, three cations of La3+, Gd3+, and Yb3+ (corresponding to large, medium and small cations, respectively) were placed in the A-site of the AZO compounds through co-precipitation–calcination technique at 1000°C for 3 h to achieve LaZO: La2Zr2O7, GdZO: Gd2Zr2O7, and YbZO: Yb2Zr2O7, respectively. The phase stability of LaZO, GdZO, and YbZO was assessed under 50 h of heat treatment at 1300°C. Characterization techniques such as conventional and high-temperature XRD, Raman and Fourier transform infrared (FTIR) spectroscopies, simultaneous thermal analysis (DTA/TG), and field-emission scanning electron microscopy (FESEM) were employed to assess the synthesized compounds. FESEM results of LaZO, GdZO and YbZO calcinated powders indicated orderly particles, uniform in shape and size, with a relative tendency of agglomeration and with an average particle size of less than ∼100 nm. XRD results of LaZO and YbZO powders after calcination indicated the formation of pyrochlore and defect fluorite structures, respectively. The placement of Gd3+ (GdZO) led to the formation of a dual pyrochlore-defect fluorite structure. The current research also indicated an enhancement in the tendency to form pyrochlore structure in GdZO and YbZO compounds along with the growth of the grains after 20 (mean grain size of ∼250 nm) and 50 h (mean grain size of ∼800 nm) of exposure to the temperature of 1300°C, respectively.