Rapid synthesis process and characterization for high purity sodium thioantimoniate nonahydrate

For the first time, Na₃SbS₄·9H₂O, also known as Schlippe's salt, has been synthesized through high-energy ball milling. This innovative synthesis way allows for obtaining high purity thioantimonate nonahydrate with around 90% yield in only approximately four hours. To validate the synthesis route described herein, the crystal structure has been refined, at room temperature, through high-resolution X-ray diffraction, pair distribution function analysis and energy dispersive spectrometry. Dehydration and rehydration of the compound have also been studied by thermogravimetric analysis and differential scanning calorimetry.