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We studied the influence of the ethylenediaminetetraacetic acid (EDTA) content used as combustion fuel when fabricating nickel oxide (NiO) nanocatalysts via solution combustion synthesis, as well as the growth behavior of carbon nanotubes (CNTs) using this catalyst. Nickel nitrate hexahydrate (Ni(NO3)2∙6H2O) was used as the metal precursor (an oxidizer), and the catalysts were synthesized by adjusting the molar ratio of fuel (EDTA) to oxidizer in the range of 1:0.25 to 2.0. The results of the crystal structure analysis showed that as the EDTA content increased beyond the chemical stoichiometric balance with Ni(NO3)2∙6H2O (F/O = 0.25), the proportion of Ni metal within the catalyst particles decreased, and only single-phase NiO was observed. Among the synthesized catalysts, the smallest crystallite size was observed with a 1:1 ratio of Ni ions to EDTA. However, an increase in the amount of EDTA resulted in excessive fuel supply, leading to an increase in crystallite size. Microstructure analysis revealed porous NiO agglomerates due to the use of EDTA, and differences in particle growth based on the fuel ratio were observed. We analyzed the growth behavior of CNTs grown using NiO nanocatalysts through catalytic chemical vapor deposition (CCVD). As the F/O ratio increased, it was observed that the catalyst particles grew excessively beyond hundreds of nanometers, preventing further CNT growth and leading to a rapid termination of CNT growth. Raman spectroscopy was used to analyze the structural characteristics of CNTs, and it was found that the ID/IG ratio indicated the highest CNT crystallinity near an F/O ratio of 1:1.

The effects of CaO content and post-heat treatment were investigated on the phase stability and mechanical and thermal properties of Ca-PSZ. ZrO2 specimens with 5–10 mol% CaO were sintered, and post-heat treatment was performed at 1200 °C for 100 h. Subsequently, to test and analyze the crystal structure and the microstructure, the mechanical and thermal properties of the specimens were evaluated. All specimens were partially stabilized by 5–10 mol% CaO (5CSZ–10CSZ) in a mixed monoclinic and tetragonal phase; however, peaks of the secondary phase of CaZrO3 were observed in 10CSZ. The ratio of the monoclinic phase decreased from 62.50% (5CSZ) to 21.02% (10CSZ) as the CaO content increased. Additionally, the monoclinic phase ratio decreased from 59.38% (5CSZ) to 19.57% (9CSZ) after the post-heat treatment; an increase to 24.84% was observed for 10CSZ. An increase in Vickers hardness from 676.02 to 1256.25 HV and flexural strength from 437.7 to 842.7 MPa was observed with increasing CaO content. The post-heat treatment resulted in further increases in these values as the CaO content increased from 5CSZ to 9CSZ; however, the Vickers hardness and flexural strength of 10CSZ decreased by approximately 8% and 9%, respectively. The thermal expansion coefficient exhibited the same tendency as the mechanical properties. This coefficient increased from 8.229 × 10−6 to 9.448 × 10−6 K−1 with increasing CaO content and was enhanced after the post-heat treatment in 5CSZ to 9CSZ; however, the thermal expansion coefficient of 10CSZ decreased by approximately 4% after the post-heat treatment. The mechanically and thermally stable tetragonal phase increased, and the monoclinic phase decreased as the doped Ca replaced the Zr sites, as was confirmed by the X-ray diffraction (XRD) analysis. The post-heat treatment and the increased Ca addition further facilitated the replacement of Zr sites by Ca. However, at high Ca concentrations of 10CSZ, an equilibrium phase of CaZrO3 was formed as a secondary phase at the post-heat treatment temperature, resulting in low performance.

The phase formation and stabilization behaviors of calcia partially stabilized zirconia (Ca-PSZ) were investigated with regard to the CaO content and post-heat treatment. Sintered specimens were prepared by adding 2, 3, 4, and 5 mol% to CaO to ZrO2, and post-heat treatment were conducted. In the X-ray diffraction pattern, the monoclinic peak decreased, the tetragonal peak increased upon CaO doping, and no CaZrO3 peak was observed. Transmission electron microscopy images of the Ca-PSZ showed that the d-spacing of 4CSZ (200)m extended from 0.260 nm to 0.266 nm subsequent to post-heat treatment. The coefficient of thermal expansion gradually increased in accordance with the dopant concentration, in addition, it increased even after the post-heat treatment. These results are related to the increase in tetragonal phase, which has a relatively higher coefficient of thermal expansion than that of the monoclinc phase. According to the Vickers hardness measurement, the hardness of all specimens increased gradually as the concentration of CaO increased, and the hardness of the 5CSZ was improved from 676 to 774 Hv by the post-heat treatment.