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Energies 2022, 15, 6452 6 of 21 kept at each temperature for 15 min, during which 15 consecutive scans were performed between 27◦ and 33◦ with a scanning step of 0.017◦ to investigate the evolution of the monoclinic and tetragonal phases. The temperature was increased at a rate of 50 ◦C/min. The crystallinity of the produced ZrOx thin films on silicon substrates annealed at 350 ◦C was also investigated using the same XRD equipment in grazing incidence mode (GIXRD, X’Pert PRO PANalytical) with a step of 0.2◦/min and an angle of incidence of the X-ray beam fixed at 0.5◦ in the range of 10–60◦ (2θ). SEM images were acquired using a Hitachi Regulus 8220 Scanning Electron Microscope (Mito, Japan) equipped with energy dispersive X-ray spectroscopy (EDS) equipment. For the FIB experiments, a Carl Zeiss AURIGA CrossBeam (FIB-SEM) workstation (Carl Zeiss MicrosPANI/TiO2 copy GmbH, Oberkochen, Germany) was used. The inner structure of the ZrO2 capacitor was observed by FIB, where Ga+ ions were accelerated to 30 kV at 50 pA, and the etching depth was maintained at around 500 nm. TEM observations were performed with a Hitachi HF5000 field-emission transmission electron microscope (Mito, Japan) operated at 200 kV. A drop of the sonicated dispersions was deposited onto 200-mesh lacey-carbon copper grids and allowed to dry before observation. The average particle size and standard deviation were calculated from the dimensions of 50 nanoparticles with ImageJ software based on TEM images. Raman spectroscopy measurements were conducted with an inVia Qontor confocal Raman microscope from Renishaw (Kingswood, UK). A 50 mW green diode operated at 532 nm was used as the excitation source, with an exposure time of 10 s and settings of 3 and 7 accumulations for ZrO2 nanopowders before and after annealing treatment, respectively. The laser beam was focused with a long working distance (8.2 mm) 50 × Olympus objective and a 100 × Olympus objective with 0.35 mm working distance, respectively, for the samples before and after annealing treatment. The Raman spectra were recorded in the range of 110–800 cm−1 (as an extended scan). Several scans on different points of the ZrO2 nanopowder’s surface were recorded, and the present results are based on their average. Possible fluctuations of the Raman equipment were avoided with a previous calibration with a silicon wafer (521 cm−1 peak). All Raman measurements were performed at ambient conditions. RT PL and PLE measurements were carried out in the microwave synthesized ZrO2 nanopowders, before and after calcination, using a Fluorolog-3 Horiba Scientific set-up with a double additive grating Gemini 180 monochromator (1200 gr/mm and 2 × 180 mm) in the excitation and a triple grating iHR550 spectrometer in the emission (1200 gr/mm and 550 mm). A 450 W Xe lamp was used as the excitation source, and different excitation wavelengths were explored. The PLE data was obtained by monitoring the maximum of the PL emission. The electrical and dielectric properties such as capacitance-voltage (C − V), capacitance- frequency (C − f) and current-voltage (I − V) measurements of the MIS capacitors ZrOx- based were investigated by using a semiconductor parameter analyzer (Keysight B1500A) with a probe station (Cascade EPS150 Triax). 3. Results and Discussion 3.1. Structural and Optical Characterization of the ZrO2 Nanopowders Produced under Microwave Irradiation 3.1.1. Raman Spectroscopy Measurements ZrO2 nanopowder was synthesized through a hydrothermal method assisted by microwave irradiation. Raman spectroscopy measurements were performed to investigate the crystalline phase of the synthesized ZrO2 nanoparticles [76]. A further calcination process was also carried out at 800 ◦C for 15 min. Figure 2a,b show the Raman spectra in the 110–800 cm−1 range for the synthesized ZrO2 nanopowders before and after the calcination treatment, respectively. Regarding the as-synthesized ZrO2 powder, as seen in Figure 2a, broader Raman bands were observed when a comparison was made with the calcinated material (Figure 2b) [77]. Nevertheless, some of the peak positions of thePDF Image | Comparison between Solution-Based Synthesis Methods of ZrO2
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