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Oxyhydrides – Synthesis, Crystal Structure and Properties

Fjellvåg, Øystein Slagtern
Doctoral thesis
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PhD-Fjellvåg-2019.pdf (12.31Mb)
Year
2019
Permanent link
http://urn.nb.no/URN:NBN:no-72400

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  • Kjemisk institutt [825]
Abstract
This thesis focus on the research of the new and scarcely explored material class oxyhydrides, where the anionic lattice consists of both oxide and hydride anions. Selected oxyhydrides described by the formula La2‑xNdxLiHO3 (0 ≤ x ≤ 2) have been obtained by a halide salt flux method in large quantities (gram scale). We describe key factors for preparation of oxyhydrides by this approach, and we discover lithium chloride to serve as an excellent flux also below its melting temperature, opening for a completely new temperature range for synthesis of oxyhydrides. Phase pure Nd2LiHO3 was in this work produced phase pure for the first time. Neutron diffraction was employed to study the long range and local structure of La2LiHO3, and neutron spectroscopy combined with computational methods yields new insight the migration of hydride anions in the compound based on evaluation of the chemical bonding.

LaSr3Fe3O9 is found to be a new layered compound with a G-type antiferromagnetic structure which is immiscible with LaSr3Fe3O10‑δ. Preliminary neutron diffraction experiments on corresponding oxyhydrides prepared by topotactic anion-exchange with CaH2, indicate successful preparation of an oxyhydride with the composition LaSr3Fe3H1.1O8.9.
List of papers
Paper I: Thermal and Structural Aspect of the Hydride Conducting Oxyhydride La2LiHO3 obtained via a Halide Flux Method ØS Fjellvåg, J Armstrong, WA Sławiński, AO Sjåstad Inorganic Chemistry, 2017, 56, 11123-11128. The paper is removed from the thesis in DUO due to publisher restrictions. The published version is available at: https://doi.org/10.1021/acs.inorgchem.7b01409
Paper II: Advances on the LiCl salt flux method and the preparation of phase pure La2-xNdxLiHO3 (0 ≤ x ≤ 2) oxyhydrides ØS Fjellvåg, KH Nygård, P Vajeeston, AO Sjåstad Chemical Communications, 2019, 55, 3817-3820. The published version of the article is included in the thesis. Also available at: https://doi.org/10.1039/C9CC00920E
Paper III: New Insights into Hydride Bonding, Dynamics and Migration in La2LiHO3 Oxyhydride ØS Fjellvåg, J Armstrong, P Vajeeston, AO Sjåstad The Journal of Physical Chemistry Letters, 2018, 9, 353-358. The paper is removed from the thesis in DUO due to publisher restrictions. The published version is available at: https://doi.org/10.1021/acs.jpclett.7b03098
Paper IV: Crystal structure of LaSr3Fe3O9 and its phase relation with LaSr3Fe3O10 ØS Fjellvåg, V Øygarden, MH Sørby, AO Sjåstad Journal of Solid State Chemistry, 2019, 275, 56-62. The published version of the article is included in the thesis. Also available at: https://doi.org/10.1016/j.jssc.2019.03.050
 
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