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Impact of cation redox chemistry on continuous hydrothermal synthesis of 2D-Ni(Co/Fe) hydroxides

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Abstract

Continuous hydrothermal flow synthesis (CHFS) is a facile, upscalable and cost-efficient synthetic method enabling the nanostructuring of advanced functional materials in steady conditions, i.e. not in batch synthesis. In this paper, we use CHFS to crystallize NiCo- and NiFe-hydroxides in water solution with 2D nanofeatures. By tuning the synthetic parameters, we disclose the key role of the cation redox chemistry in the transition between two competitive phases: from 2D-nanoplatelets of brucite to layered double hydroxides (LDH). For controlling the precipitation of different Ni, Fe, Co-hydroxide phases, we propose the combined use of an oxidizing (H2O2) and a complexing (NH3) agent. At temperatures as low as 80 °C, the presence of H2O2 and a low concentration of NH3 favour the Ni2+/Co3+ over Ni2+/Co2+ oxidation states, shifting the product structure from brucite phase (temperatures > 80 °C) to LDH. Conversely, for the NiFe-hydroxides the transition from LDH (temperatures ≤ 80 °C) to brucite phase (temperatures > 80 °C) is controlled by the reaction temperature only. Due to the high stability of Fe3+, the synthesis of NiFe products by CHFS does not require oxidizing and complexing agents, resulting in a robust process for large-scale production.

Graphical abstract: Impact of cation redox chemistry on continuous hydrothermal synthesis of 2D-Ni(Co/Fe) hydroxides

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Publication details

The article was received on 14 Aug 2019, accepted on 08 Oct 2019 and first published on 08 Oct 2019


Article type: Paper
DOI: 10.1039/C9RE00334G
React. Chem. Eng., 2019, Advance Article

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    Impact of cation redox chemistry on continuous hydrothermal synthesis of 2D-Ni(Co/Fe) hydroxides

    M. Rosa, D. Marani, G. Perin, S. B. Simonsen, P. Zielke, A. Glisenti, R. Kiebach, A. Lesch and V. Esposito, React. Chem. Eng., 2019, Advance Article , DOI: 10.1039/C9RE00334G

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