Synthesis of morphologically different SnHPO 4 using a refluxing method

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This work presents a simple and efficient reflux method for the synthesis of Tin(II) hydrogen phosphate (SnHPO4). This method is faster and requires less instrumentation. The reported methods use highly hygroscopic SnCl2 as the starting material, whereas the current method uses more stable SnO. The synthesised SnHPO4 was characterised by powder X-ray diffraction (PXRD), FTIR spectroscopy, Raman spectroscopy and thermal gravimetry (TG). PXRD confirmed the formation of crystalline SnHPO4 with no detectable secondary phases, while FTIR and Raman spectroscopy verified the characteristic phosphate and hydroxyl vibrations. TG analysis demonstrated the thermal stability of SnHPO4 up to approximately 300°C, followed by dehydration and phase transformation at higher temperatures. Chemical methods were used to confirm the oxidation state of Sn and the Sn:P ratio in the synthesised SnHPO4. The effect of using different recrystallising solvents on the final yield, shape and size of SnHPO4 particles was investigated using scanning electron microscopy (SEM) and static light scattering (SLC) techniques. Acetone, acetonitrile, hexane, and water were used as the recrystallising solvents. Different recrystallising solvents produced significant differences in particle morphology and particle-size distribution. Hexane resulted in the highest product recovery. Crystals formed by using acetonitrile appear as small granular aggregates, while those from hexane appear as large flat plate-like crystals.