High-pressure X-ray and Raman study of a ferrian magnesian spodumene

The high-pressure behaviour of a synthetic P21/c ferrian magnesian spodumene, M2 (Li0.85Mg0.09Fe2+ 0.06)M1(Fe3+ 0.85Mg0.15)Si2O6, has been investigated using in situ single-crystal X-ray diffraction and Raman spectroscopy. No phase transition has been observed within the pressure range investigated. The isothermal equation of state up to 7 GPa was determined. V0, KT0 and K’, simultaneously refined with a Murnaghan equation of state, are: V0= 415.66(7) A3, KT0=83(1) GPa and K’=9.6(6). The magnitudes of the principal unit-strain coefficients were calculated and their ratios e1:e2:e3=1.00:1.85:2.81 at P=6.83 GPa indicate a very strong anisotropy. Monitoring of the intensity of b-type reflections (h+k= 2n+1) confirms that from room conditions up to 7 GPa the primitive lattice is maintained. Raman spectra have been collected up to 7.4 GPa. No change in the number of observed vibrational modes occurs in the pressure range investigated. At high frequency, the Raman doublet relative to the Si–O–Si vibrations of the two distinct tetrahedral chains is a broad band at room pressure, however, the frequency difference between the two modes increases with increasing pressure.