Cold sintering of whitlockite-based phosphate ceramics for ALPS carbonate slurry waste immobilization

Gubarevich, A.*; Kubo, Ryotaro*; Arisaka, Makoto ; Osugi, Takeshi  ; Yoshida, Katsumi*; Takeshita, Kenji*

To immobilize and solidify carbonate-based Advanced Liquid Processing System (ALPS) sediment wastes, this study introduces a chemical transformation process that converts these wastes into calcium and magnesium phosphate phases, followed by densification using a novel cold sintering press (CSP) technique. Simulated calcium-magnesium carbonate slurries were treated with phosphoric acid to synthesize calcium and magnesium phosphates, which were then sintered at 300-500C using CSP. The effects of the calcium-to-magnesium ratio, strontium incorporation, and sodium chloride addition on phase composition and CSP densification were investigated. Dense bulk samples were successfully fabricated and characterized using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and the Archimedes method. The results showed that the chemical transformation process led to the formation of whitlockite and newberyite, with the calcium-to-magnesium ratio determining the relative proportions of these phases. Strontium was effectively incorporated into the whitlockite crystal structure, while newberyite enhanced densification through a dehydration-driven process. Sodium chloride had no effect on chemical transformation and was not found in the final solid product. These results show that direct conversion of calcium-magnesium carbonate slurries to whitlockite-based phosphate ceramics, followed by CSP, enables stable solidification, making this method promising for ALPS sediment waste management.