Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

On the Rehydration of Organic Layered Double Hydroxides to Form Graphene-LDH Nanocomposites

Version 1 : Received: 22 July 2018 / Approved: 23 July 2018 / Online: 23 July 2018 (12:02:37 CEST)

A peer-reviewed article of this Preprint also exists.

Conterosito, E.; Palin, L.; Antonioli, D.; Riccardi, M.P.; Boccaleri, E.; Aceto, M.; Milanesio, M.; Gianotti, V. On the Rehydration of Organic Layered Double Hydroxides to form Low-Ordered Carbon/LDH Nanocomposites. Inorganics 2018, 6, 79. Conterosito, E.; Palin, L.; Antonioli, D.; Riccardi, M.P.; Boccaleri, E.; Aceto, M.; Milanesio, M.; Gianotti, V. On the Rehydration of Organic Layered Double Hydroxides to form Low-Ordered Carbon/LDH Nanocomposites. Inorganics 2018, 6, 79.

Abstract

A graphene-containing LDH was prepared by re-hydration of the oxides produced by the calcination of an organic LDH. While the memory effect is a widely recognized effect on oxides produced by inorganic LDHs, it is unprecedented from the calcination/re-hydration of organic ones. Different temperatures (400, 600 and 1100 °C) were tested, on the basis of thermogravimetric data. Water instead of a carbonate solution was used for the re-hydration, with CO2 available from water itself and/or air to induce a slower process with an easier and better intercalation of the carbonaceous species within the layers. The samples were characterized by X-ray Powder Diffraction (XRPD), IR and Raman spectroscopy and scanning electron microscopy (SEM). XRPD indicate the presence of carbonate LDH mixed with a layered phase with a larger d-spacing. IR confirmed that the prevailing anion is carbonate, coming from the water used for the re-hydration and/or air. Raman data indicated the presence of low-ordered graphenic species moieties and SEM the absence of separated graphene of graphitic sheets, suggesting an intimate mixing of the carbonaceous phase with reconstructed LDH. Organic LDHs gave better memory effect after calcination at 400 °C. Conversely, the graphenic species are observed after rehydration of the sample calcined at 600 °C with a reduced memory effect, demonstrating the interference of the carbonaceous phase with LDH reconstruction and the bonding with LDH layers to form a graphene-LDH nanocomposite.

Keywords

layered double LDHs; graphene; mixed oxides; re-hydration; memory Effect; X-ray diffraction; Raman spectroscopy; scanning electron microscopy

Subject

Chemistry and Materials Science, Nanotechnology

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