Synthesis, structural characterization and high pressure phase transitions of monolithium hydronium sulfate
- Synthesis, structural characterization and high pressure phase transitions of monolithium hydronium sulfate
- D. banerjee; A. M. Plonka; 김선진; W. Xu; J. B. parise
- High pressure; Crystal structure; Phase transition; Monolithium sulfate; Monolithium; Single crystalX-raydiffraction; Sulfate; High pressure Raman spectroscopy; Solvothermal; Temperature dependent XRD
- Issue Date
- Journal of solid state chemistry
- VOL 197, 181-185
- A three dimensional lithium hydronium sulfate LiSO4·H3O , [space group Pna21 a=8.7785(12) Å, b=9.1297(12) Å, c=5.2799(7) Å, V=423.16(10) Å3] was synthesized via solvothermal methods using 1,5-naphthalenedisulfonic acid (1,5-NSA) as the source of sulfate ions. The structure of , determined by single crystal X-ray diffraction techniques, consists of corner sharing LiO4 and SO4 tetrahedra, forming an anionic 3-D open framework that is charge balanced by hydronium ions positioned within channels running along  and forming strong H-bonding with the framework oxygen atoms. Compound  undergoes two reversible phase transitions, involving reorientation of SO42− ions at pressures of approximately 2.5 and 5 GPa at room temperature, as evident from characteristic discontinuous frequency drops in the ν1 mode of the Raman spectra. Additionally, compound  forms dense β-lithium sulfate at 300 °C, as evident from temperature dependent powder XRD and combined reversible TGA-DSC experiments.
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