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Quasielastic neutron scattering with in situ
control: Water dynamics in uranyl fluoride
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The structural phase diagram of uranyl fluoride
(UO2F2), while incomplete, contains at least one anhydrous
structure and a second, zeolite-like structure with the
[(UO2F2)(H2O)]7 ⋅ (H2O)4
that can be produced by adding water to the anhydrous structure. While traditional diffraction
easily differentiate these crystals, additional aqueous structures (in general
of the form UO2F2 + xH2O) have been proposed as well. We
present results using a novel sample environment setup to intercalate waterduring a quasielastic neutron scatteringmeasurement over
the course of 86 h. Our sample environment allows low-pressure (<2 atm) humid air flow
across the sample coupled with a system to control the relative humidity of this air flow
between 10% and 70%. The water dynamics in UO2F2 and
[(UO2F2)(H2O)]7 ⋅ (H2O)4
are sufficiently different to distinguish them, with water in the latter executing
a restricted diffusion (D = 2.7 × 10−6 cm2/s)
within the structure's accessible pores (r = 3.17 Å) such that
the dynamics can be used as a fingerprinting tool. We confirm that water vaporpressure is the
driving thermodynamic force for the conversion of the anhydrous structure to
[(UO2F2)(H2O)]7 ⋅ (H2O)4,
and we demonstrate the feasibility of extending this approach to aqueous forms of
UO2F2 + xH2O. This method has general applicability to
systems in which water content itself is a driving variable for structural or dynamical
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