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Energies 2022, 15, 6452 16 of 21 Figure 11c shows a typical current density versus breakdown field dependence. The results are in accordance with solution-based ZrOx thin film capacitors [71]. Once low leakage current density was reached (<10−5 A/cm2), it opens the window for future applications such as gate insulators for solution-based thin film transistors. 4. Conclusions This work demonstrated that both the hydrothermal method assisted by microwave irradiation and solution combustion synthesis are reliable and simple production routes for ZrO2 nanomaterials, including nanoparticles and thin films. Moreover, the low-cost character of the study is evidenced by the inexpensive apparatus required to produce and deposit ZrOx thin films and thus fabricate energy storage devices. In both synthesis routes, XRD analysis revealed that the as-synthesized powders had a mixture of ZrO2 monoclinic and tetragonal phases. A calcination treatment at 800 ◦C for 15 min was imposed on the microwave synthesized nanopowder to promote the conversion into single- phase materials. Nevertheless, in situ XRD and TEM analysis revealed a minor presence of the ZrO2 tetragonal phase after the calcination treatment. Different nanostructures were observed after synthesis in both production routes. In the case of the microwave synthesized material, after calcination, near-spherical nanoparticles were observed, while plate-like structures composed of nano-sized grains were identified for the combustion synthesis. The effect of calcination on the optical properties of the microwave synthesized nanopowders was evaluated by PL and PLE, showing a clear broadening and an increased intensity of the ZrO2 band observed in the visible spectral region after calcination. This band was tentatively associated with the presence of oxygen vacancy-related defects. Solution combustion synthesis also resulted in thin films, and XRD analysis suggested their amorphous nature. SEM and FIB measurements of the ZrOx capacitors revealed that the thin films present a thickness of 14.2 ± 0.1 nm, which leads to a dielectric constant of 11.0 ± 0.5 (calculated at 1 kHz). The devices also presented a good breakdown field of 2.8 ± 0.1 MV/cm and a low leakage current density of (3.9 ± 1.1) × 10−7 A/cm2 at 1 MV/cm. From this study, the production of ZrO2 nanomaterials with two simple, cost- effective and easily upscaling synthesis routes and their integration on capacitors can be highlighted. Supplementary Materials: The following supporting information can be downloaded at: https:// www.mdpi.com/article/10.3390/en15176452/s1, Figure S1: High-resolution TEM image of the ZrO2 nanocrystals calcinated at 800 ◦C for 15 min. The inset shows the FFT images of the area (black square) indicated as A; Figure S2: SEM image of a ZrO2 particle produced by solution combustion synthesis and annealed at 350 ◦C. Author Contributions: M.L.M. was responsible for producing and characterizing microwave synthe- sized materials, as well as writing the manuscript. H.d.V. was responsible for the production and characterization of the ZrOx films, and J.M. was responsible for the combustion powder synthesis. M.M. and A.P. were responsible for the XRD measurements. D.N., R.B. and E.C. were responsible for the overall scientific orientation and revising the manuscript. D.N. performed the TEM observations and analysis. T.M. and J.R. were responsible for the optical measurements, respective analyses and revising of the manuscript. E.F. and R.M. were responsible for supervising all the processes and obtaining funding. Part of the work resulted from the Master of Science thesis of H.d.V., titled: Effect of eco-friendly solvents in solution-based ZrOx dielectrics, developed at the Nova School of Science and Technology. All authors have read and agreed to the published version of the manuscript. Funding: This work was financed by national funds from FCT-Fundação para a Ciência e a Tecnologia, I.P., in the scope of the projects UI/BD/151292/2021 (Ph.D. research scholarship), LA/P/0037/2020, UIDP/50025/2020 and UIDB/50025/2020 of the Associate Laboratory Institute of Nanostructures, Nanomodelling and Nanofabrication-i3N, but also the 2021.03825.CEECIND. The work was also partially funded by the Nanomark collaborative project between INCM (Imprensa Nacional-Casa da Moeda) and CENIMAT/i3N. Acknowledgments also go to the EC project SYNERGY H2020- WIDESPREAD-2020-5, CSA, proposal n◦ 952169, EMERGE-2020-INFRAIA-2020-1, proposal n◦PDF Image | Comparison between Solution-Based Synthesis Methods of ZrO2
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