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energies Article A Comparison between Solution-Based Synthesis Methods of ZrO2 Nanomaterials for Energy Storage Applications Maria Leonor Matias 1 , Emanuel Carlos 1,* , Rita Branquinho 1 , Hadassa do Valle 1, João Marcelino 1, Maria Morais 1 , Ana Pimentel 1, Joana Rodrigues 2 , Teresa Monteiro 2 , Elvira Fortunato 1, Rodrigo Martins 1,* and Daniela Nunes 1,* 1 2 * Correspondence: e.carlos@fct.unl.pt (E.C.); rm@uninova.pt (R.M.); daniela.gomes@fct.unl.pt (D.N.); Tel.: +351-21-294-8562 (R.M. & D.N.); Fax: +351-21-294-8558 (R.M. & D.N.) Abstract: The present study is focused on the synthesis of zirconium dioxide (ZrO2) nanomaterials using the hydrothermal method assisted by microwave irradiation and solution combustion synthesis. Both synthesis techniques resulted in ZrO2 powders with a mixture of tetragonal and monoclinic phases. For microwave synthesis, a further calcination treatment at 800 ◦C for 15 min was carried out to produce nanopowders with a dominant monoclinic ZrO2 phase, as attested by X-ray diffraction (XRD) and Raman spectroscopy. The thermal behavior of the ZrO2 nanopowder was investigated by in situ XRD measurements. From the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images, the presence of near spherical nanoparticles was clear, and TEM confirmed the ZrO2 phases that comprised the calcinated nanopowders, which include a residual tetragonal phase. The optical properties of these ZrO2 nanopowders were assessed through photoluminescence (PL) and PL excitation (PLE) at room temperature (RT), revealing the presence of a broad emission band peaked in the visible spectral region, which suffers a redshift in its peak position, as well as intensity enhancement, after the calcination treatment. The powder resultant from the solution combustion synthesis was composed of plate-like structures with a micrometer size; however, ZrO2 nanoparticles with different shapes were also observed. Thin films were also produced by solution combustion synthesis and deposited on silicon substrates to produce energy storage devices, i.e., ZrO2 capacitors. The capacitors that were prepared from a 0.2 M zirconium nitrate-based precursor solution in 2-methoxyethanol and annealed at 350 ◦C exhibited an average dielectric constant (κ) of 11 ± 0.5 and low leakage current density of 3.9 ± 1.1 × 10−7 A/cm2 at 1 MV/cm. This study demonstrates the simple and cost-effective aspects of both synthesis routes to produce ZrO2 nanomaterials that can be applied to energy storage devices, such as capacitors. Keywords: ZrO2; nanomaterials; microwave irradiation; solution combustion; energy storage devices 1. Introduction Research in nanotechnology has grown over in recent years since it opens up possibili- ties for the design and fabrication of novel materials, as well as flexible and smart devices at the nanometer scale [1,2]. In this regard, nanostructures based on metal oxides have been extensively studied due to their unique physical and chemical properties and great potential in a myriad of applications, including electronics, energy conversion and storage, biomedicine, catalysis and sensing [3–8]. ZrO2 is a metal oxide that exhibits three crystalline phases under atmospheric pressure, depending on the synthesis route: monoclinic, which is thermodynamically the most stable form [9], tetragonal and cubic [10–12]. The cubic form of ZrO2 is stable at high temperatures (usually above 2370 ◦C), while the tetragonal is stable within the range of 1170–2370 ◦C, and the monoclinic phase stabilizes below 1170 ◦C [4,9]. CENIMAT|i3N, Department of Materials Science, School of Science and Technology, NOVA University Lisbon and CEMOP/UNINOVA, 2829-516 Caparica, Portugal Physics Department & I3N, Aveiro University, Campus Universitário de Santiago, 3810-193 Aveiro, Portugal Citation: Matias, M.L.; Carlos, E.; Branquinho, R.; do Valle, H.; Marcelino, J.; Morais, M.; Pimentel, A.; Rodrigues, J.; Monteiro, T.; Fortunato, E.; et al. A Comparison between Solution-Based Synthesis Methods of ZrO2 Nanomaterials for Energy Storage Applications. Energies 2022,15,6452. https://doi.org/ 10.3390/en15176452 Academic Editors: Bruno Peuportier and Zsuzsa Szalay Received: 26 July 2022 Accepted: 31 August 2022 Published: 3 September 2022 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). Energies 2022, 15, 6452. https://doi.org/10.3390/en15176452 https://www.mdpi.com/journal/energiesPDF Image | Comparison between Solution-Based Synthesis Methods of ZrO2
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