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Energies 2022, 15, 6452 Energies 2022, 15, x FOR PEER REVIEW 14 of 21 15 of Figure 9. TEM images of the ZrO powder produced with solution combustion synthesis and Figure 9. TEM ima2ges of the ZrO2 powder produced with solution combustion synthesis and ◦ resolution TEM images of the ZrO2 nanocrystals. The inset in (b) shows the FFT images of the a (b) high-resolution TEM images of the ZrO2 nanocrystals. The inset in (b) shows the FFT images of annealed in air atn3ea5l0ed Cin faoira1t 3h5.0 °(Ca)foBrr1igh.t-(afi)eBldrigThEt-MfielidmTaEgMe oimf athge oZfrtOhe ZnraOn2onpaanrotpicalretsiclaensdand (b) hi 2 3.2.3. ZrOx Thin Films X-ray DiffractionX-ray Diffraction (black square) indicated as C. the area (black square) indicated as C. 3.2.3. ZrOx Thin Films The ZrOx thin films were produced with the same solution used for producing t The ZrOx thin films were produced with the same solution used for producing the ZrO2 powder by solution combustion. Spin coating was employed to deposit ZrOx t ZrO2 powder by solution combustion. Spin coating was employed to deposit ZrOx thin films on silicon substrates to be tested as capacitors. Crystalline dielectric films may p films on silicon substrates to be tested as capacitors. Crystalline dielectric films may provide, vide, for instance, pathways for leakage current due to the grain boundaries, which resu for instance, pathways for leakage current due to the grain boundaries, which results in a in a small on/off ratio, leading to poor capacitor performance. On the contrary, amorpho small on/off ratio, leading to poor capacitor performance. On the contrary, amorphous thin thin films have a smooth surface, high stability, low interface state density, as well films have a smooth surface, high stability, low interface state density, as well as large-area large-area uniformity [100,101]. uniformity [100,101]. Grazing angle mode was performed to analyze the crystalline structure of ZrOx t Grazing angle mode was performed to analyze the crystalline structure of ZrOx thin films annealed at 350 °C in air for 30 min on a hot plate. An annealing treatment at 350 films annealed at 350 ◦C in air for 30 min on a hot plate. An annealing treatment at 350 ◦C was carried out since it was reported that annealing treatments in solution-process was carried out since it was reported that annealing treatments in solution-processed high-κ high-𝜅 ZrOx thin films between 300–600 °C are expected to increase O−2 content in Zr ZrOx thin films between 300–600 ◦C are expected to increase O−2 content in ZrOx films, films, leading to a reduction of oxygen defects and/or hydroxyl groups and consequen leading to a reduction of oxygen defects and/or hydroxyl groups and consequently of of conduction paths [69,102]. conduction paths [69,102]. As observed in Figure 10, some diffraction maxima are visible at 2θ = 51.4° and 2 As observed in Figure 10, some diffraction maxima are visible at 2θ = 51.4◦ and 53.4°, accompanied by a bump at around 55° (2θ), which correspond to forbidden diffr 2θ = 53.4◦, accompanied by a bump at around 55◦ (2θ), which correspond to forbidden tion planes of a (100)-oriented silicon wafer that appear when the grazing angle mode diffractionplaneussoedfat(c1e0r0ta)-ionrpiehnitaendglseil[i1c0o3n].wApaafertrftrhoamttahpapt,enaorowtherndtifhfreagctriaoznimngaxainmgalewereiden mode is used at cfeiertda,iindpihciatainglteh[e1a0m3]o. rApphoaurtsfnroatmurtehoaft,thneoportohdeurcdeidffZrarcOtixotnhimn faixlmims,awheicrhe is ideal identified, indicatihning ftihlme acmapoarcpihtoruaspnpalitcuarteioonfs.the produced ZrOx thin films, which is ideal for thin film capacitor applications. 3.3. Electrical Characterization of the ZrOx Capacitors ZrOx thin films were implemented in metal-insulator-semiconductor (MIS) devices to evaluate their dielectric performance. Figure 11a show the typical C–V curve of the ZrOx thin film capacitors with a small hysteresis. The devices present good stability with a small change of the capacitance over the frequency (1 kHz–100 kHz), as depicted in Figure 11b. To calculate the dielectric contact, a cross-section of the device to deter- mine the ZrOx thickness was performed, as shown in the inset of Figure 11b. The ZrOx thin films present a capacitance per unit area of 672 ± 28 nF cm−2 and a dielectric con- stant of 11.0 ± 0.5 (both calculated at 1 kHz). These values are lower when compared with vacuum deposited crystalline films due to the lower film density and presence of pores as a consequence of the solution process [71,72,104–106]. Nevertheless, the devices a g r h r h ° O t θ a fPDF Image | Comparison between Solution-Based Synthesis Methods of ZrO2
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