Synchrotron single-crystal XRD, IR-, Raman spectroscopy and high pressure study of synthetic krieselite

• Published in: Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy Vol. 288; p. 122137
• Main Authors: Borovikova, E.Yu, Spivak, A.V., Setkova, T.V., Kvas, P.S., Kuzmin, A.V., Zakharchenko, E.S., Balitsky, V.S., Khasanov, S.S., Lazarenko, V.A., Dorovatovskii, P.V., Korshunov, D.M., Aksenov, S.M.
• Format: Journal Article
• Language: English
• Published: England Elsevier B.V 05.03.2023
• Subjects: FTIR; High pressure; Krieselite; Raman spectroscopy; Synthesis; Topaz; Synthesis; Raman spectroscopy; Topaz; FTIR; Krieselite; High pressure
• ISSN: 1386-1425; 1873-3557
• DOI: 10.1016/j.saa.2022.122137

[Display omitted] •Krieselite was synthesized at 600 °C and 100 MPa by hydrothermal method.•Single crystal structure was refined by XRD.•The assignment of Ag bands in non-polarized Raman spectra was carried out.•Lattice dynamic calculations agree with experimental Raman data.•Krieselite Raman spectra are obtained as function of pressure up to 30 GPa. Spontaneous crystals of krieselite (Ge analogue of topaz) with the chemical formula Al2[(Ge0.75Si0.25)O4](F1.63OH0.37) were synthesized using a thermo-gradient hydrothermal method at a temperature of 600/650 °C and pressure of 100 MPa. The unit cell parameters are: a = 8.9732(8) Å, b = 8.4823(7) Å, c = 4.7379(5) Å, V = 360.62(6) Å3, space group Pnma. The F-/OH– content of the samples was refined by FTIR spectroscopy method. Raman spectroscopy showed the main differences between the spectra of krieselite and topaz at the ambient conditions. The assignment of observed and calculated Ag bands (cm−1) for non-polarized Raman spectra was carried out. Using in situ Raman spectroscopy at high pressures, the dependence of the shift in the position of the main bands of the krieselite Raman spectrum on the pressure was established, and the corresponding paths of pressure induced distortion of crystal structure was assumed. According to the data of Raman spectroscopy, it was revealed that krieselite does not undergo the phase transitions up to 30 GPa. The probable way of crystal structure distortion within the space group Pnma was proposed based on simulation of high-pressure Raman spectra.