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@ARTICLE{Magro:903599,
author = {Magro, Fernando and Ceretti, Monica and Meven, Martin and
Paulus, Werner},
title = {{I}nfrared furnace for in situ neutron single-crystal
diffraction studies in controlled gas atmospheres at high
temperatures},
journal = {Journal of applied crystallography},
volume = {54},
number = {3},
issn = {0021-8898},
address = {[S.l.]},
publisher = {Wiley-Blackwell},
reportid = {FZJ-2021-05253},
pages = {822 - 829},
year = {2021},
abstract = {For the understanding of oxygen diffusion mechanisms in
non-stoichiometric oxides, the possibility to explore
structural changes as a function of the oxygen partial
pressure with temperature and related oxygen bulk
stoichiometry is mandatory. We report here on the
realization of a high temperature furnace, suitable for
single crystal neutron diffraction, working continuously at
temperatures up to 1000°C at different and adjustable
partial gas pressures up to 2 bars. This allows to explore
the phase diagrams of non-stoichiometric oxides under in
operando conditions under controlled oxygen partial
pressure. As a pilot study we explored the structural
changes of Pr$_2$NiO$_{4+\delta}$ at room temperature
($\delta$ ≈ 0.24), and at 900°C under 1 bar P(O2)
($\delta$ ≈ 0.13) as well as under secondary vacuum
(approximately 10$^{-5}$ mbar) condition yielding a $\delta$
close to zero. The strong anharmonic displacements of the
apical oxygen atoms along the [110] shallow diffusion
pathway, which were previously observed at RT and 400°C,
clearly become more isotropic at 900°C. Our study evidences
that the anisotropic oxygen displacements, here related to
lattice instabilities, play a major role to understand
oxygen diffusion pathways and related activation energies at
moderate temperatures. This also shows the importance of the
availability of such reaction cells for single crystal
neutron diffraction to explore the phase diagram and
associated structural changes of non-stoichiometric oxygen
ion conductors and respective diffusion mechanisms.},
cin = {JCNS-FRM-II / MLZ / JARA-FIT / JCNS-2 / PGI-4},
ddc = {540},
cid = {I:(DE-Juel1)JCNS-FRM-II-20110218 / I:(DE-588b)4597118-3 /
$I:(DE-82)080009_20140620$ / I:(DE-Juel1)JCNS-2-20110106 /
I:(DE-Juel1)PGI-4-20110106},
pnm = {6G4 - Jülich Centre for Neutron Research (JCNS) (FZJ)
(POF4-6G4) / 632 - Materials – Quantum, Complex and
Functional Materials (POF4-632)},
pid = {G:(DE-HGF)POF4-6G4 / G:(DE-HGF)POF4-632},
experiment = {EXP:(DE-MLZ)HEIDI-20140101},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000659339200011},
doi = {10.1107/S1600576721003198},
url = {https://juser.fz-juelich.de/record/903599},
}