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Energies 2022, 15, 6452 13 of 21 3.2.2. Electron Microscopy Figure 8 shows the SEM images of the ZrO2 powder resultant from the solution com- bustion synthesis. The formation of micro-sized plate-like structures is clear, as seen in Figure 8a. Nevertheless, Figure 8b indicates the presence of nano-sized grains composing the micro-sized structure, and Figure S2 suggests the stacking of several nanolayers. In- dividual nanoparticles were also observed. Moreover, the void-like nature of the particle observed in Figure S2 can be associated with the escape of gaseous combustion products that were formed during combustion synthesis [58]. EDS measurements were also carried out, and, as observed for the ZrO2 nanoparticles produced under microwave irradiation Energies 2022, 15, x FOR PEER REVIEW 14 of 23 (Figure 4), the presence of a homogeneous distribution of Zr (Figure 8c) and O (Figure 8d) was clear. No impurities were detected by this technique. Figure 8. (a,b) SEM images of the ZrO particle produced by the combustion synthesis method and Figure 8. (a,b) SEM images of the ZrO22particle produced by the combustion synthesis method and ◦ aafftteerrannealliinginairat350 °Cfforr11hh,,totoggeeththererwwitihththtehecocrorrersepsopnodnidnignEgDESDmSampasposfZofrZ(cr)(acn)danOd(dO). (d). The atomic percentages of Zr and O were also estimated by EDS point analysis (Table 2). As observed for the nanopowders synthesized under microwave irradiation, the values The atomic percentages of Zr and O were also estimated by EDS point analysis (Table were within the expected range for pure zirconium oxide (the Zr/O ratio was 1:2.1). 2). As observed for the nanopowders synthesized under microwave irradiation, the values were within the expected range for pure zirconium oxide (the Zr/O ratio was 1:2.1). Table 2. EDS point analysis of the ZrO2 nanopowder produced by the solution combustion synthesis. Table 2. EDS point analysis of the ZrO2 nanopowder produced by the solution combustion synthe- sis. Elements Zr at.% 31.9 Elements at.% O 68.1 68.1 The ZrO2 powder produced by solution combustion synthesis was also observed by TEM, confirming the presence of individual ZrO2 nanoparticles. From Figure 9a, nano-sized The ZrO2 powder produced by solution combustion synthesis was also observed by particles with different shapes can be observed, including nanospheres, nano squares and TEM, confirming the presence of individual ZrO2 nanoparticles. From Figure 9a, nano- irregular-shaped nanoparticles (Figure 9a). Larger particles without a specific shape were sized particles with different shapes can be observed, including nanospheres, nano also observed; nevertheless, the average particle size was 10 ± 7 nm. The lattice spacing of squares and irregular-shaped nanoparticles (Figure 9a). Larger particles without a specific 0.3 nm was measured on an individual ZrO2 nanoparticle (Figure 9b), which was consistent shape were also observed; nevertheless, the average particle size was 10 ± 7 nm. The lattice with the d-spacing of the (101) plane of the tetragonal ZrO2. Nonetheless, as observed by spacing of 0.3 nm was measured on an individual ZrO2 nanoparticle (Figure 9b), which XRD results, the powder was a mixture of tetragonal and monoclinic ZrO2 phases. was consistent with the d-spacing of the (101) plane of the tetragonal ZrO2. Nonetheless, as observed by XRD results, the powder was a mixture of tetragonal and monoclinic ZrO2 phases. Zr 31.9 OPDF Image | Comparison between Solution-Based Synthesis Methods of ZrO2
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