Solid‐state mixed ionic–electronic conductors (MIECs) in which ionic transport is commonly accompanied by predominant electronic conductivity underpin key technologies and require universal characterization methods for monitoring transport at the nanoscale, at both high and near ambient temperatures, the latter being especially challenging. In this study, a novel dynamic current–voltage analysis technique is utilized to decouple ionic and electronic transport properties from each other. The versatility of the method is demonstrated by enabling measurement of the oxygen vacancy mobility in Pr0.1Ce0.9O2−δ thin films, across an unusually wide temperature range, from 35 to 500 °C. Despite the presence of predominant electronic conduction, the oxygen vacancy mobility in Pr0.1Ce0.9O2−δ is measured, being 6.8 × 10−6 cm2 V−1 s−1 at 500 °C, decreasing by seven orders of magnitude down to 35 °C, and following a single thermal activation energy of 0.82 ± 0.02 eV. A comparison with previous reports on oxygen vacancy transport and with the one derived in this study from impedance spectroscopy, interpreted with the Jamnik–Maier model, further confirms the dynamic current–voltage analysis results. This method can more generally be applied to other types of MIECs, thereby enabling deeper insights into mobile ionic defect transport and accompanying thermodynamic properties.
In this study, an approach to characterize ceramic colloidal suspensions has been developed, based on vitrification of aqueous ceramic suspensions and microstructural characterization using cryogenic-temperature scanning electron microscopy (cryo-SEM), augmented by conventional rheological measurements. The flocculation phenomenon in as-milled and aged Mg-spinel (MgAl 2 O 4 ) aqueous suspensions was characterized. A microstructure based on hard particle agglomerates separated by long-chain deflocculant molecules was directly observed, and correlated to the rheological properties of the suspension. Several levels of flocculation were detected as a function of suspension preparation conditions. Although suspensions at solid-loading levels appropriate for ceramic processing cannot be characterized using conventional particle size measurement techniques, cryo-SEM can be used to measure characteristic sizes, and to distinguish between agglomerated and flocculated particles, opening a new approach for optimizing solid-loading conditions for slip casting in terms of viscosity and green density.
Vacuum-deposited perovskites provide a more direct path to manufacturing large area solar cells because of ready compatibility with multilayered architectures and historic use in the electronics industry. However, vacuum compatible co-deposition of organic-inorganic perovskites remains difficult due to issues of precisely controlling the organic precursor flux. Here, we demonstrate a manufacturing prototype specifically designed for co-depositing organic-inorganic perovskites and evaluate it with respect to the influence of process parameters on film growth. Through depositing and characterizing methylammonium lead iodide (MAPbI3) perovskite films, we highlight the necessary design requirements while measuring the influence of film growth parameters on deposition rate and perovskite phases.
Solid state mixed ionic-electronic conductors in which ionic transport is commonly accompanied by predominant electronic conductivity, underpin key technologies and require universal characterization methods for monitoring transport at the nanoscale, at both high and near ambient temperatures, the latter being especially challenging. In this study, a novel dynamic current-voltage analysis technique is utilized to decouple ionic and electronic transport properties from each other. The versatility of the method is demonstrated by enabling measurement of the oxygen vacancy mobility in Pr0.1Ce0.9O2-δ thin films, across an unusually wide temperature range, from 35 to 500 °C. Despite the presence of predominant electronic conduction, the oxygen vacancy mobility in Pr0.1Ce0.9O2-δ was measured, being 6.8×10-6 cm2V-1s-1 at 500 °C, decreasing by seven orders of magnitude down to 35 °C, and following a single thermal activation energy of 0.82 ± 0.02 eV. A comparison with previous reports on oxygen vacancy transport and with the one derived in this study from impedance spectroscopy, interpreted with the Jamnik-Maier model, further confirms the dynamic current-voltage analysis results. This method can more generally be applied to other types of mixed ionic-electronic conductors, thereby enabling deeper insights into mobile ionic defect transport and accompanying thermodynamic properties.
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