| Summary: | This paper reports on the preparation of xenotime-structured ceramics using the Spark Plasma Sintering (SPS) method. Y<sub>0.95</sub>Gd<sub>0.05</sub>PO<sub>4</sub> (YPO<sub>4</sub>:Gd) phosphates were obtained using the sol-gel method. The synthesized powders were nanodispersed and were agglomerated (the agglomerates sizes were 10–50 µm). The ceramics had a fine-grained microstructure and a high relative density (98.67 ± 0.18%). The total time of the SPS process was approximately 18 min. The sintered high-density YPO<sub>4</sub>:Gd ceramics with a xenotime structure were irradiated with <sup>132</sup>Xe<sup>+26</sup> ions with 167 MeV of energy and fluences in the range of 1 × 10<sup>12</sup>–3 × 10<sup>13</sup> cm<sup>−2</sup>. Complete amorphization was not achieved even at the maximum fluence. The calculated value of the critical fluence was (9.2 ± 0.1) × 10<sup>14</sup> cm<sup>−2</sup>. According to the results of grazing incidence X-ray diffraction (GIXRD), the volume fraction of the amorphous structure increased from 20 to 70% with increasing fluence from 1 × 10<sup>12</sup> up to 3 × 10<sup>13</sup> cm<sup>−2</sup>. The intensity of the 200 YPO<sub>4</sub>:Gd XRD peak reached ~80% of the initial intensity after recovery annealing (700 °C, 18 h).
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