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Solid solution along the synthetic LiAISi2O6-LiFeSi2O6 (spodumene-ferri-spodumene) join: A general picture of solid solutions, bond lengths, lattice strains, steric effects, symmetries, and chemical compositions of Li clinopyroxenes

  • Gianluca Iezzi EMAIL logo , Geoffrey D. Bromiley , Andrea Cavallo , Partha P. Das , Fotini Karavassili , Irene Margiolaki , Andrew A. Stewart , Mario Tribaudino and Jonathan P. Wright
Published/Copyright: October 29, 2016
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American Mineralogist
From the journal American Mineralogist Volume 101 Issue 11

Abstract

Seven clinopyroxene compositions along the join M2LiM1AlTSi2O6 (spodumene) to M2LiM1Fe3+TSi2O6 (ferri-spodumene) were synthesized at 2 GPa, 800 °C under highly oxidizing conditions (using H2O2 fluid) in an end-loaded piston cylinder. In addition, the LiFe3+Si2O6 composition was also synthesized under the intrinsically reducing conditions in a piston cylinder, to check the effect of fO2 on iron speciation. The run products were characterized by field emission scanning electron microscope (FE-SEM), Rietveld refinements on XRPD synchrotron data, and space groups were assigned using SAED-TEM patterns. Run products are composed mainly of lithium clinopyroxene (Li-Cpx), plus minor amounts of hematite (magnetite under reducing condition) and corundum, as independently detected by image analysis (area%) and Rietveld refinements (wt%); moreover, Rietveld results were used to derive cell parameters, M1-site occupancy (Al vs. Fe3+), atomic positions, and average bond lengths of all these Li-Cpx indexed in the C2/c space groups according to SAED-TEM.

Li-Cpx with Al and Fe3+ amounts close to 50:50 are actually slightly richer in Al apfu than nominal; the LiFe3+Si2O6 grown under very oxidized and reducing conditions have very similar cell parameters, indicating that fO2 is unable to induce a significant incorporation of Fe2+ in these Li-Cpx. The replacement of Al with Fe3+ induces a linear (%) increase of the cell edges following b > a > c, whereas β is roughly constant and the cell volume increases linearly. Furthermore, the substitution of Al with Fe3+ only weakly affects the T-O average length (<1%), whereas M2-O and M1-O bonds increase linearly of 2.3 and 5.0%, respectively.

These new experimental data have been compared with other available on Li-, Na-, and Ca-Cpx, i.e., M2(Li,Na,Ca,Mg,Fe2+)M1(Mg,Fe2+Al,Ni,Cr,Ga,V,Fe3+,Mn,Sc,In)TSi2O6, to model lattice strain, bond lengths, steric effects, and phase transitions behaviors. The replacement of Al with progressively larger cations in LiM3+Si2O6 Cpx (M3+: Ni, Cr, Ga, V, Fe3+, Ti, Sc, and In) results in a linear increase following V > b > a > c, whereas β is roughly constant except for Ti-end-member and P21/c compositions. Lattice strains induced by X, T, and P for Li-Cpx in the C2/c stability field show that when the M1 site is progressively filled with a large cation, ε1 axis (ε1 > ε2 > ε3) increases along b, whereas ε2 and ε3 are nearly parallel to a and at about 30° from c. Conversely, T will provoke a similar enlargement of ε1 and ε2 along b and a edges, respectively, whereas ε3 is again oriented at about 30° from c; the increasing of P will instead shorten all strain tensor components (ε1, ε2, and ε3) with a similar percentage amount; notably, high-P is the only stress that induces a strain component to be almost parallel to c edge. Moreover, finite lattice strains and orientation in C2/c LiMe3+Si2O6 Li-Cpx induced by Me3+: Al-Fe3+, Fe3+-Sc, Sc-In are slightly different, with ε1 invariably lying along b; conversely, Li-Na cation substitution is completely different with the highest and lowest deformations on the ac plane and ε2 along b; ε3 vector is negative and oriented at about 30° from T-chains. The ideal replacement of Al with larger cations up to In in Li-Cpx induces the M1-O, M2-O, and T-O average bond lengths to increase by 10.6, 4.3, and <0.5%. Steric effects in LiM1Me3+Si2O6 and NaM1Me3+Si2O6 Cpx are significant and very similar, whereas several other Me1+ and Me2+ substitutions in Cpx at both the M1 and M2 site, keeping fixed the other site, display less or even the absence of steric effects. Our new data also better elucidate relationships between Li-Cpx composition, symmetry at room and non-ambient conditions and Tc. The aggregate cation radii at the M1 site does not exclusively control the stability of C2/c and P21/c polymorphs; instead valence electrons can profoundly favor the stabilization of a polymorph.

Acknowledgments

We warmly acknowledge the editorial handling of the D.G. Gatta, the fruitful suggestions of the Crystal Structures Editor R.J. Angel that deeply enhanced the presentation of crystallographic data. We strongly appreciate the revisions of G.J. Redhammer and an anonymous reviewer that enhanced the clarity of this study.

We thank the interdepartmental laboratory of Electron Microscopy and Microanalysis, located at the Biology Department of Patras University (Greece), for access to equipment and technical assistance. We also thank NanoMEGAS SPRL (Belgium) for technical support and funding for the research work related to Transmission Electron Microscopy. G.I. was supported by the “Fondi Ateneo of the University G. d’Annunzio of Chieti.”

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Received: 2016-3-24
Accepted: 2016-6-27
Published Online: 2016-10-29
Published in Print: 2016-11-1

© 2016 by Walter de Gruyter Berlin/Boston

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https://doi.org/10.2138/am-2016-5784

Articles in the same Issue

  1. Highlights and Breakthroughs
  2. Melts, mush, and more: Evidence for the state of intermediate-to-silicic arc magmatic systems
  3. Investigating petrologic indicators of magmatic processes in volcanic rocks
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  11. Special Collection: Apatite: A Common Mineral, Uncommonly Versatile
  12. U-Pb LA-ICP-MS dating of apatite in mafic rocks: Evidence for a major magmatic event at the Devonian-Carboniferous boundary in the Armorican Massif (France)
  13. Special Collection: Apatite: A Common Mineral, Uncommonly Versatile
  14. Quantification of CO2 concentration in apatite
  15. Special Collection: Apatite: a Common Mineral, Uncommonly Versatile
  16. Phosphate minerals in the H group of ordinary chondrites, and fluid activity recorded by apatite heterogeneity in the Zag H3-6 regolith breccia
  17. Special Collection: Apatite: A Common Mineral, Uncommonly Versatile
  18. In situ elemental and isotopic analysis of fluorapatite from the Taocun magnetite-apatite deposit, Eastern China: Constraints on fluid metasomatism
  19. Special Collection: Geology and Geobiology of Lassen Volcanic National Park
  20. Acido-thermotolerant fungi from Boiling Springs Lake, LVNP: Potential for lignocellulosic biofuels
  21. Research Article
  22. Solid solution along the synthetic LiAISi2O6-LiFeSi2O6 (spodumene-ferri-spodumene) join: A general picture of solid solutions, bond lengths, lattice strains, steric effects, symmetries, and chemical compositions of Li clinopyroxenes
  23. Research Article
  24. Formation of hydrous stishovite from coesite in high-pressure hydrothermal environments
  25. Research Article
  26. Raman characterization of synthetic magnesian calcites
  27. Research Article
  28. Yangite, PbMnSi3O8·H2O, a new mineral species with double wollastonite silicate chains, from the Kombat mine, Namibia
  29. Research Article
  30. Ideal wollastonite and the structural relationship between the pyroxenoids and pyroxenes
  31. Research Article
  32. Influence of the octahedral cationic-site occupancies on the framework vibrations of Li-free tourmalines, with implications for estimating temperature and oxygen fugacity in host rocks
  33. Research Article
  34. In situ X-ray observation of 10 Å phase stability at high pressure
  35. Research Article
  36. New mineral names
  37. Book Review
  38. Book Review: Pore-Scale Geochemical Processes, RIMG Volume 80
  39. Book Review
  40. Book Review: Highly Siderophile and Strongly Chalcophile Elements in High-Temperature Geochemistry and Cosmochemistry, RIMG Volume 81
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