Synthesis, structural characterization and high pressure phase transitions of monolithium hydronium sulfate

Title
Synthesis, structural characterization and high pressure phase transitions of monolithium hydronium sulfate
Authors
D. banerjeeA. M. Plonka김선진W. XuJ. B. parise
Keywords
High pressure; Crystal structure; Phase transition; Monolithium sulfate; Monolithium; Single crystalX-raydiffraction; Sulfate; High pressure Raman spectroscopy; Solvothermal; Temperature dependent XRD
Issue Date
2013-01
Publisher
Journal of solid state chemistry
Citation
VOL 197, 181-185
Abstract
A three dimensional lithium hydronium sulfate LiSO4·H3O [1], [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 [1], 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 [001] and forming strong H-bonding with the framework oxygen atoms. Compound [1] 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 [1] forms dense β-lithium sulfate at 300 °C, as evident from temperature dependent powder XRD and combined reversible TGA-DSC experiments.
URI
http://pubs.kist.re.kr/handle/201004/45099
ISSN
00224596
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KIST Publication > Article
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