Journal of Solid State Chemistry, volume 230, pages 266-271
The solubility and site preference of Fe3+ in Li7−3Fe La3Zr2O12 garnets
Daniel Rettenwander
1
,
Charles A. Geiger
1
,
M. Tribus
2
,
Peter Tropper
2
,
R. Wagner
1
,
G. Tippelt
1
,
W. Lottermoser
1
,
G. Amthauer
1
1
Department of Materials Research and Physics, University of Salzburg , 5020 Salzburg, Austria.
|
Publication type: Journal Article
Publication date: 2015-10-01
Journal:
Journal of Solid State Chemistry
Quartile SCImago
Q2
Quartile WOS
Q2
Impact factor: 3.3
ISSN: 00224596, 1095726X
Materials Chemistry
Ceramics and Composites
Electronic, Optical and Magnetic Materials
Inorganic Chemistry
Physical and Theoretical Chemistry
Condensed Matter Physics
Abstract
A series of Fe3+-bearing Li7La3Zr2O12 (LLZO) garnets was synthesized using solid-state synthesis methods. The synthetic products were characterized compositionally using electron microprobe analysis and inductively coupled plasma optical emission spectroscopy (ICP-OES) and structurally using X-ray powder diffraction and 57Fe Mössbauer spectroscopy. A maximum of about 0.25 Fe3+ pfu could be incorporated in Li7-3x Fe x La3Zr2O12 garnet solid solutions. At Fe3+ concentrations lower than about 0.16 pfu, both tetragonal and cubic garnets were obtained in the synthesis experiments. X-ray powder diffraction analysis showed only a garnet phase for syntheses with starting materials having intended Fe3+ contents lower than 0.52 Fe3+ pfu. Back-scattered electron images made with an electron microprobe also showed no phase other than garnet for these compositions. The lattice parameter, a0, for all solid-solution garnets is similar with a value of a0≈12.98 Å regardless of the amount of Fe3+. 57Fe Mössbauer spectroscopic measurements indicate the presence of poorly- or nano-crystalline FeLaO3 in syntheses with Fe3+ contents greater than 0.16 Fe3+ pfu. The composition of different phase pure Li7-3x Fe x La3Zr2O12 garnets, as determined by electron microprobe (Fe, La, Zr) and ICP-OES (Li) measurements, give Li6.89Fe0.03La3.05Zr2.01O12, Li6.66Fe0.06La3.06Zr2.01O12, Li6.54Fe0.12La3.01Zr1.98O12, and Li6.19Fe0.19La3.02Zr2.04O12. The 57Fe Mössbauer spectrum of cubic Li6.54Fe0.12La3.01Zr1.98O12 garnet indicates that most Fe3+ occurs at the special crystallographic 24d position, which is the standard tetrahedrally coordinated site in garnet. Fe3+ in smaller amounts occurs at a general 96h site, which is only present for certain Li-oxide garnets, and in Li6.54Fe0.12La3.01Zr1.98O12 this Fe3+ has a distorted 4-fold coordination.
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Rettenwander D. et al. The solubility and site preference of Fe3+ in Li7−3Fe La3Zr2O12 garnets // Journal of Solid State Chemistry. 2015. Vol. 230. pp. 266-271.
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Rettenwander D., Geiger C. A., Tribus M., Tropper P., Wagner R., Tippelt G., Lottermoser W., Amthauer G. The solubility and site preference of Fe3+ in Li7−3Fe La3Zr2O12 garnets // Journal of Solid State Chemistry. 2015. Vol. 230. pp. 266-271.
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TY - JOUR
DO - 10.1016/j.jssc.2015.01.016
UR - https://doi.org/10.1016/j.jssc.2015.01.016
TI - The solubility and site preference of Fe3+ in Li7−3Fe La3Zr2O12 garnets
T2 - Journal of Solid State Chemistry
AU - Rettenwander, Daniel
AU - Geiger, Charles A.
AU - Tribus, M.
AU - Tropper, Peter
AU - Wagner, R.
AU - Tippelt, G.
AU - Lottermoser, W.
AU - Amthauer, G.
PY - 2015
DA - 2015/10/01 00:00:00
PB - Elsevier
SP - 266-271
VL - 230
SN - 0022-4596
SN - 1095-726X
ER -
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@article{2015_Rettenwander,
author = {Daniel Rettenwander and Charles A. Geiger and M. Tribus and Peter Tropper and R. Wagner and G. Tippelt and W. Lottermoser and G. Amthauer},
title = {The solubility and site preference of Fe3+ in Li7−3Fe La3Zr2O12 garnets},
journal = {Journal of Solid State Chemistry},
year = {2015},
volume = {230},
publisher = {Elsevier},
month = {oct},
url = {https://doi.org/10.1016/j.jssc.2015.01.016},
pages = {266--271},
doi = {10.1016/j.jssc.2015.01.016}
}