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Open AccessArticle

Bimodal Porosity and Stability of a TiO2 Gig-Lox Sponge Infiltrated with Methyl-Ammonium Lead Iodide Perovskite

National Research Council-Institute for Microelectronics and Microsystems (CNR-IMM), Zona Industriale-Strada VIII n°5, 95121 Catania, Italy
Department of Mathematical and Computational Sciences, Physics and Earth Sciences, University of Messina, Viale F. Stagno d’Alcontres 31, 98166 Messina, Italy
ESRF, The European Synchrotron, CS40220, 38043 Grenoble CEDEX 9, France
Institut Matériaux Microélectronique Nanosciences de Provence (IM2NP) Aix-Marseille Université, 13397 Marseille CEDEX 20, France
Author to whom correspondence should be addressed.
Nanomaterials 2019, 9(9), 1300;
Received: 2 August 2019 / Revised: 31 August 2019 / Accepted: 6 September 2019 / Published: 11 September 2019
We created a blend between a TiO2 sponge with bimodal porosity and a Methyl-Ammonium Lead Iodide (MAPbI3) perovskite. The interpenetration of the two materials is effective thanks to the peculiar sponge structure. During the early stages of the growth of the TiO2 sponge, the formation of 5–10 nm-large TiO2 auto-seeds is observed which set the micro-porosity (<5 nm) of the layer, maintained during further growth. In a second stage, the auto-seeds aggregate into hundreds-of-nm-large meso-structures by their mutual shadowing of the grazing Ti flux for local oxidation. This process generates meso-pores (10–100 nm) treading across the growing layer, as accessed by tomographic synchrotron radiation coherent X-ray imaging and environmental ellipsometric porosimetry. The distributions of pore size are extracted before (>47% V) and after MAPbI3 loading, and after blend ageing, unfolding a starting pore filling above 80% in volume. The degradation of the perovskite in the blend follows a standard path towards PbI2 accompanied by the concomitant release of volatile species, with an activation energy of 0.87 eV under humid air. The use of dry nitrogen as environmental condition has a positive impact in increasing this energy by ~0.1 eV that extends the half-life of the material to 7 months under continuous operation at 60 °C. View Full-Text
Keywords: Ti-oxides; perovskites; blend; nano-scale; sputtering; Thornton; shadowing Ti-oxides; perovskites; blend; nano-scale; sputtering; Thornton; shadowing
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Sanzaro, S.; Zontone, F.; Grosso, D.; Bottein, T.; Neri, F.; Smecca, E.; Mannino, G.; Bongiorno, C.; Spinella, C.; La Magna, A.; Alberti, A. Bimodal Porosity and Stability of a TiO2 Gig-Lox Sponge Infiltrated with Methyl-Ammonium Lead Iodide Perovskite. Nanomaterials 2019, 9, 1300.

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